The title compound 1,2-bis(1-phenyl-3-methylthio-4-iminopyrazolo[3,4-d] pyrimidin-5-yl)ethane (C26H24N10S2, Mr = 540.67) was obtained by the reaction of (1-phenyl-4- cyano)pyrazol-5-yliminomethyl ethyl ether with ethy...The title compound 1,2-bis(1-phenyl-3-methylthio-4-iminopyrazolo[3,4-d] pyrimidin-5-yl)ethane (C26H24N10S2, Mr = 540.67) was obtained by the reaction of (1-phenyl-4- cyano)pyrazol-5-yliminomethyl ethyl ether with ethyldiamine. The crystal is monoclinic, space group P21/c with a = 10.460(2), b = 8.004(2), c =15.434(3) ? b = 90.803(3)? V = 1292.1(4) 3, Z = 2, Dc = 1.390 g/cm3, F(000) = 564, m(MoKa) = 0.24 mm-1, R = 0.0560 and wR = 0.1344 for 2286 observed reflections (I > 2s (I)). In this compound the dihedral angle between the plane defined by C(2), N(1), N(2), C(3), C(6), N(3), C(4), N(4), C(5) and N(5) atoms and the phenyl ring is 34.78? The six-membered ring consisted of C(3), N(3), C(4), N(4), C(5) and C(6) atoms forms a p67 configuration in which the N(4) atom is sp2 hybrid. There exist weak hydrogen bonds between S(1) and N(5) atoms (NHS, 3.430 ?.展开更多
Continuous homogenous azeotropic distillation(CHAD) and pressure-swing distillation(PSD) are explored to separate a minimum-boiling azeotropic system of ethyl acetate and n-hexane. The CHAD process with acetone as the...Continuous homogenous azeotropic distillation(CHAD) and pressure-swing distillation(PSD) are explored to separate a minimum-boiling azeotropic system of ethyl acetate and n-hexane. The CHAD process with acetone as the entrainer and the PSD process with the pressures of 0.1 MPa and 0.6 MPa in two columns are designed and simulated by Aspen Plus. The operating conditions of the two processes are optimized via a sequential modular approach to obtain the minimum total annual cost(TAC). The computational results show that the partially heat integrated pressure-swing distillation(HIPSD) has reduced in the energy cost and TAC by 40.79% and 35.94%, respectively, than the conventional PSD, and has more greatly reduced the energy cost and TAC by 62.61% and 49.26% respectively compared with the CHAD process. The comparison of CHAD process and partially HIPSD process illustrates that the partially HIPSD has more advantages in averting the product pollution, energy saving, and economy.展开更多
The experiment aimed to evaluate the effects of N and trinexapac-ethyl (TE) to the growth of Kentucky bluegrass. By using the method of randomized blocks design, 4 N levels, 0 (N1), 20 (N2), 25 (N3), and 30 ...The experiment aimed to evaluate the effects of N and trinexapac-ethyl (TE) to the growth of Kentucky bluegrass. By using the method of randomized blocks design, 4 N levels, 0 (N1), 20 (N2), 25 (N3), and 30 (N4) kg N ha t mon% with TE at 0 (T1), 312.5 (T2) and 625 (T3) mL ha-1 every 10 d effect on the total height, clippings and chlorophyll concentration of Kentucky bluegrass were evaluated. Results showed that total height and total clippings of Kentucky bluegrass were reduced by treating with TE and increased by treating with N. Kentucky bluegrass treated with 312.5 and 625 mL ha ' per 10 d had total clippings and total height reduced 30 and 45% under different N application level. The N × TE interaction was significant for the chlorophyll concentration of Kentucky bluegrass. The chlorophyll concentration of Kentucky bluegrass treated with TE at 625 mL ha-1 every 10 d was significantly higher than that of Kentucky bluegrass treated with 312.5 mL ha-1 every 10 d at the same N level. The chlorophyll concentration of turfgrass treated with TE at 625 mL ha-1 every 10 d receiving 30 kg N ha -1 month-1 was the highest. Based on the index of turf growth and the chlorophyll concentration, turfgrass receiving 20 or 30 kg N ha-1 month-1 with 625 mL TE ha i every 10 d could balance the problem of mowing frequency and growth quickly while keeping a good quality.展开更多
Hydrogenation of carbazole and N-ethylcarbazole over Raney-Ni catalyst were realized in the temperature range of 393-503 K. 4[H] adduct dominated the hydrogenation products and the formation of 2[H] adduct was the rat...Hydrogenation of carbazole and N-ethylcarbazole over Raney-Ni catalyst were realized in the temperature range of 393-503 K. 4[H] adduct dominated the hydrogenation products and the formation of 2[H] adduct was the rate-limiting step during the period, in which the conversion of carbazole was less than 40%. The hydrogenation process followed pseudo-first-order kinetics and the hydrogenation activation energies of carbazole and N-ethylcarbazole were 90 kJ/mol and 115 kJ/mol, respectively. The reaction starting position as well as the pathway of the hydrogenation of (N-ethyl)carbazole were investigated by comparing the kinetic characteristics of hydrogen uptake of carbazole and N- ethylcarbazole. The results showed that the reaction was a stepwise hydrogenation process and the first H_2 was added to the C1 = C10 double bond in the hydrogenation.展开更多
A kinetic model was developed to describe the atom transfer radical polymerization (ATRP) of 2-(N,N-dimethylamino) ethyl methacrylate (DMAEMA). The model was based on a polymerization mechanism,which included the atom...A kinetic model was developed to describe the atom transfer radical polymerization (ATRP) of 2-(N,N-dimethylamino) ethyl methacrylate (DMAEMA). The model was based on a polymerization mechanism,which included the atom transfer equilibrium for primary radical, the propagation of growing polymer radical, and the atom transfer equilibrium for the growing polymer radical. An experiment was carried out to measure the conversion of monomer, the number-average molecular weight of polymer and molecular weight distribution for the ATRP process of DMAEMA. The experimental data were used to correlate the kinetic model and rate constants were obtained. The rate constants of activation and deactivation in the atom transfer equilibrium for primary radical are 1.0×10^4L·mol^-1·s^-1 and 0.04L·mol^-1·s^-1, respectively. The rate constant of the propagation of growing polymer radical is 8.50L·mol^-1·s^-1, and the rate constants of activation and deactivation in the atom transfer equilibrium for growing polymer radical are 0.045L·mol^-1·s^-1 and 1.2×10^5L·mol^-1·s^-1, respectively. The values of the rate constants represent the features of the ATRP process. The kinetic model was used to calculate the ATRP process of DMAEMA. The results show that the calculations agree well with the measurements.展开更多
Reactive dividing-wall column(RDWC) technology plays a critical role in the energy saving and high efficiency of chemical process.In this article, the process of co-producing ethyl acetate(EA) and n-butyl acetate(BA) ...Reactive dividing-wall column(RDWC) technology plays a critical role in the energy saving and high efficiency of chemical process.In this article, the process of co-producing ethyl acetate(EA) and n-butyl acetate(BA) with RDWC was studied.BA was not only the product, but also acted as entrainer to remove the water generated by the two esterification reactions.Experiments and simulations of the co-production process were carried out.It was found that the experimental results were in good agreement with the simulation results.Two kinds of RDWC structures(RDWC-FC and RDWC-RS) were proposed, and the co-production process operating parameters of the two types of RDWC were optimized by Aspen Plus respectively.The optimal operating parameters of the RDWC-FC were determined as follows: 0.6 of the reflux ratio of aqueous phase(RR), 0.66 of the vapor split(R_V) and 0.51 of the liquid split(R_L).And the optimal operating parameters of the RDWC-RS were shown as follows: RR was 0.295 and R_V was 0.61.Furthermore, the energy saving analysis of the co-production process was based on the annual output of 10000 tons of EA, compared with the traditional reaction distillation(RD) to prepare EA and BA, the reboiler duty of the RDWC-FC column could save 20.4%, TAC saving 23.6%; RDWC-RS reboiler energy consumption could save 17.0%, TAC 22.2%.展开更多
2-Cetyl-3-20 keto acid(N-ethyl perfluorinated octyl sulfonamide) N-ethyl ester was synthesized by the reaction of N-ethyl-N-hydroxyethyl perfluorinated octyl sulfonamide and alky ketene dimer. The experimental resul...2-Cetyl-3-20 keto acid(N-ethyl perfluorinated octyl sulfonamide) N-ethyl ester was synthesized by the reaction of N-ethyl-N-hydroxyethyl perfluorinated octyl sulfonamide and alky ketene dimer. The experimental results show that the yield of products can be 89% when the molar ratio of perfluorinated octyl sulfonamide to ketene dimer is 1 : 1.1 and the reaction lasts about four hours at 80 ℃. The structure of the product was characterized by FTIR and ^1HNMR. The product can dissolve in polar solvents such as NMP, DMAC, THF, DMSO, CHCl3, and 10% weight-loss temperature measured by TGA is 202℃.展开更多
The title compound N-2-thiophenesulfonyl-a-L-phenylalanine ethyl ester has been synthesized. Complete assignments were achieved by IR, MS, ^1H NMR and single-crystal X-ray diffraction analyses. Using MTT assay, the in...The title compound N-2-thiophenesulfonyl-a-L-phenylalanine ethyl ester has been synthesized. Complete assignments were achieved by IR, MS, ^1H NMR and single-crystal X-ray diffraction analyses. Using MTT assay, the inhibitory rate of the title compound on K562 cells (chronic myeloid leukemic cells) was measured and the result of preliminary bioassay showed that the title compound possesses antiproliferation effects on K562 cells. In order to investigate the relationship between structure and activity of the target compound, we report its crystal structure and biological behavior in the present paper. Crystallographic data: C15H17NO4S2, Mr = 339.42, monoclinic, space group P21, flack = -0.15(12), a = 5.7916(10), b = 11.5078(19), c = 12.924(2) A, β = 97.781(3)°, Z = 2, V = 853.4(2) A^3, De = 1.321 g/cm^3, F(000) = 356, -7≤h≤7, -10≤k≤14, -15 ≤ l≤15, R = 0.0628, wR = 0.1540 and μ(MoKa) = 0.327 mm^-1. The molecule comprises a benzene and a thiofuran rings, and the intramolecular N(1)-H(1A)…O(1) makes a five-membered ring of O(1)--C(6)-C(5)--N(1)--H(1A).展开更多
The title compound, N-(2-(1H-indol-3-yl)ethyl)-2-nitroaniline(C16H15N3O2, Mr = 281.31), has been synthesized by the multicomponent reaction of milder Ullmann, and its structure was characterized by 1H NMR, 13 C NMR, I...The title compound, N-(2-(1H-indol-3-yl)ethyl)-2-nitroaniline(C16H15N3O2, Mr = 281.31), has been synthesized by the multicomponent reaction of milder Ullmann, and its structure was characterized by 1H NMR, 13 C NMR, IR, H RMS(ESI) and single-crystal X-ray diffraction. It crystallizes in monoclinic, space group I2/c with a = 15.0212(10), b = 9.4911(6), c = 20.3075(13) A, β = 100.776(7)o, V = 2844.1(3)A3, Z = 8, Dc = 1.314 g/cm3, F(000) = 1184.0, μ = 0.089 mm-1, the final R = 0.0574 and w R = 0.1688 for 1701 observed reflections(I 】 2σ(I)). X-ray analysis indicates three major N(2)–H(2)···O(2), C(13)–H(13)···O(2), N(2)–H(2)···N(3) hydrogen bonds and π-π stacking interactions in the crystal structure. The preliminary biological test shows that the title compound has a good antitumor activity against A549 in vitro with the IC50 value of 35 μmol/L.展开更多
When ethyl 3-fluoroalkyl-3-haloacrylate was treated with excess CH2N2,1-methyl-3-ethoxycarbonyl-4-fluoroalkylpyr azoles(3)and 1-methyl-5-ethoxycarbonyl-4-fluoroalkylpyrazoles(4)were obtained with a ratio of 90-95:10-5...When ethyl 3-fluoroalkyl-3-haloacrylate was treated with excess CH2N2,1-methyl-3-ethoxycarbonyl-4-fluoroalkylpyr azoles(3)and 1-methyl-5-ethoxycarbonyl-4-fluoroalkylpyrazoles(4)were obtained with a ratio of 90-95:10-5 in good yield.展开更多
A nutritional fortifier N-(1-(phenylacetyl)-L-prolyl)glycine ethyl ester(4)was successfully synthesized through two synthetic schemes and characterized by IR,^1H-NMR,^13C-NMR,elemental analysis and X-ray single-crysta...A nutritional fortifier N-(1-(phenylacetyl)-L-prolyl)glycine ethyl ester(4)was successfully synthesized through two synthetic schemes and characterized by IR,^1H-NMR,^13C-NMR,elemental analysis and X-ray single-crystal diffraction.The intermediate N-phenylacetyl-L-proline(2)was synthesized by the solid-liquid reaction of L-proline and phenylacetyl chloride directly.Compound 2(C13 H15 NO3,Mr=233.26)belongs to the orthorhombic system,space group P212121 with a=8.9468(3),b=9.3190(3),c=14.0453(4)A,V=1171.03(6)A^3,Z=4,Dc=1.323 g/cm^3,μ=0.773 mm^-1,F(000)=496.0,the final R=0.0313 and wR=0.0797 for all data.Compound 4(C17 H22 N2 O4,Mr=318.36)is of orthorhombic system,space group P212121 with a=6.5831(2),b=8.5536(2),c=28.9138(9)A,V=1628.11(8)A^3,Z=4,Dc=1.299 g/cm3,μ=0.763 mm-1,F(000)=680.0,the final R=0.0353 and wR=0.0816 for all data.展开更多
Transgenic pigs have been produced with the aim of further improving pigs in terms of economic and environmental traits, but these animals have not been allowed to enter the food chain. As an alternative approach to g...Transgenic pigs have been produced with the aim of further improving pigs in terms of economic and environmental traits, but these animals have not been allowed to enter the food chain. As an alternative approach to generating pigs with novel traits of economic importance that cannot be introduced by conventional breeding, we propose a strategy for combining in vitro mutagenesis of pig primary cells with N-ethyl-N-nitrosourea (ENU) and somatic-cell nuclear transfer (SCNT) technology. To explore the feasibility of this strategy, we treated pig primary fibroblast cells with ENU, estimated the per-base mutation frequency induced by the mutagen, clonally cultured about 4000 of the mutagenized cells, and screened them for mutation within the coding region of the melanocortin-4 receptor (MC4R) gene, a key gene in energy homeostasis. Through this screening, we obtained 14 cell clones, each harboring a heterozygous base change within the coding region for MC4R. Of the mutant cell clones, each of two contained a mutant allele encoding MC4R with greatly reduced receptor activity. By SCNT using these cell clones as donors, pigs harboring mutated MC4R alleles with reduced receptor activity can be produced. Our strategy for generating pigs with novel genetic traits likely will be more acceptable to the public than is the use of transgenic technology.展开更多
In this work,a calculation method of chemical kinetics was established for labeling reaction of 99mTc-N-ethyl-N2S2-memantine,a potential NMDA receptor imaging agent prepared in our laboratory.Four groups of vials (3 v...In this work,a calculation method of chemical kinetics was established for labeling reaction of 99mTc-N-ethyl-N2S2-memantine,a potential NMDA receptor imaging agent prepared in our laboratory.Four groups of vials (3 vials per group) were added with 0.02 mL (1 mg/mL) N-ethyl-N2S2Memantine,0.08 mL (40 mg/mL) GH,0.05 mL (10 mg/mL) EDTA-2Na,0.035 mL (2 mg/mL) SnF2,0.8 mL phosphate buffer(1mol/L,pH 6.5) and 37 MBq Na99mTcO4.The vials were incubated at 70℃,80℃,90℃ or 100℃.Samples were taken with capillary from the vials at 2,5,10,20,30,40 and 60min.Labeling yields were determined by TLC.Order of reaction n,rate constant k,activation energy Ea and half life t1/2 of labeling reaction were calculated with the kinetics software we compiled.Mean labeling yields of 99m Tc-N-ethyl-N2S2-memantine at 2,5,10,20,30,40 and 60min were (1) 13.5,15.7,34.0,64.8,81.9,91.4 and 95.4 at 70℃;(2) 13.2,20.5,40.1,70.0,88.2,94.5 and 95.6 at 80℃;(3) 15.6,22.9,43.7,74.3,87.2,93.4 and 96.1 at 90℃;and (4) 20.5,25.8,45.3,81.1,92.2,95.6 and 96.0 at 100℃.The other parameters were;n =1;k=0.053,0.061,0.063 and 0.076 L/min at 70℃,80℃,90℃ and 100℃,respectively;Ea=12.38 kJ/L;t1/2=13.11,11.45,11.05 and 9.07min at 70℃,80℃,90℃ and 100℃,respectively.The mean labeling yield increased with temperature and time,optimized at 100℃ and 40-60min.The concentration of 99mTc-N-ethyl-N2S2-Memantine was larger than that of Na99mTcO4,so n=1.The k increased with reaction,hence the accelerated reaction rate at higher temperatures.The labeling reaction was not so difficult because of the low Ea.The t1/2 decreased with increasing reaction temperature,hence the acceleration of labeling reaction.展开更多
基金The project was supported by the National Natural Science Foundation of China (29832025)
文摘The title compound 1,2-bis(1-phenyl-3-methylthio-4-iminopyrazolo[3,4-d] pyrimidin-5-yl)ethane (C26H24N10S2, Mr = 540.67) was obtained by the reaction of (1-phenyl-4- cyano)pyrazol-5-yliminomethyl ethyl ether with ethyldiamine. The crystal is monoclinic, space group P21/c with a = 10.460(2), b = 8.004(2), c =15.434(3) ? b = 90.803(3)? V = 1292.1(4) 3, Z = 2, Dc = 1.390 g/cm3, F(000) = 564, m(MoKa) = 0.24 mm-1, R = 0.0560 and wR = 0.1344 for 2286 observed reflections (I > 2s (I)). In this compound the dihedral angle between the plane defined by C(2), N(1), N(2), C(3), C(6), N(3), C(4), N(4), C(5) and N(5) atoms and the phenyl ring is 34.78? The six-membered ring consisted of C(3), N(3), C(4), N(4), C(5) and C(6) atoms forms a p67 configuration in which the N(4) atom is sp2 hybrid. There exist weak hydrogen bonds between S(1) and N(5) atoms (NHS, 3.430 ?.
基金Supported by the Education Foundation of Chongqing(KJ1712307)the Application Technology Research and Developments Foundation of Fuling Technology Board(FLKJ,2016ABA1026)the Young Foundation of Yangtze Normal University(2015XJXM03)
文摘Continuous homogenous azeotropic distillation(CHAD) and pressure-swing distillation(PSD) are explored to separate a minimum-boiling azeotropic system of ethyl acetate and n-hexane. The CHAD process with acetone as the entrainer and the PSD process with the pressures of 0.1 MPa and 0.6 MPa in two columns are designed and simulated by Aspen Plus. The operating conditions of the two processes are optimized via a sequential modular approach to obtain the minimum total annual cost(TAC). The computational results show that the partially heat integrated pressure-swing distillation(HIPSD) has reduced in the energy cost and TAC by 40.79% and 35.94%, respectively, than the conventional PSD, and has more greatly reduced the energy cost and TAC by 62.61% and 49.26% respectively compared with the CHAD process. The comparison of CHAD process and partially HIPSD process illustrates that the partially HIPSD has more advantages in averting the product pollution, energy saving, and economy.
基金supported by the Key International Science and Technology Cooperation Program of China(2006DFA33630)
文摘The experiment aimed to evaluate the effects of N and trinexapac-ethyl (TE) to the growth of Kentucky bluegrass. By using the method of randomized blocks design, 4 N levels, 0 (N1), 20 (N2), 25 (N3), and 30 (N4) kg N ha t mon% with TE at 0 (T1), 312.5 (T2) and 625 (T3) mL ha-1 every 10 d effect on the total height, clippings and chlorophyll concentration of Kentucky bluegrass were evaluated. Results showed that total height and total clippings of Kentucky bluegrass were reduced by treating with TE and increased by treating with N. Kentucky bluegrass treated with 312.5 and 625 mL ha ' per 10 d had total clippings and total height reduced 30 and 45% under different N application level. The N × TE interaction was significant for the chlorophyll concentration of Kentucky bluegrass. The chlorophyll concentration of Kentucky bluegrass treated with TE at 625 mL ha-1 every 10 d was significantly higher than that of Kentucky bluegrass treated with 312.5 mL ha-1 every 10 d at the same N level. The chlorophyll concentration of turfgrass treated with TE at 625 mL ha-1 every 10 d receiving 30 kg N ha -1 month-1 was the highest. Based on the index of turf growth and the chlorophyll concentration, turfgrass receiving 20 or 30 kg N ha-1 month-1 with 625 mL TE ha i every 10 d could balance the problem of mowing frequency and growth quickly while keeping a good quality.
基金supported by the National Natural Science Foundation of China(U1162127,U1462201,21076189,21476202 and 21276231)
文摘Hydrogenation of carbazole and N-ethylcarbazole over Raney-Ni catalyst were realized in the temperature range of 393-503 K. 4[H] adduct dominated the hydrogenation products and the formation of 2[H] adduct was the rate-limiting step during the period, in which the conversion of carbazole was less than 40%. The hydrogenation process followed pseudo-first-order kinetics and the hydrogenation activation energies of carbazole and N-ethylcarbazole were 90 kJ/mol and 115 kJ/mol, respectively. The reaction starting position as well as the pathway of the hydrogenation of (N-ethyl)carbazole were investigated by comparing the kinetic characteristics of hydrogen uptake of carbazole and N- ethylcarbazole. The results showed that the reaction was a stepwise hydrogenation process and the first H_2 was added to the C1 = C10 double bond in the hydrogenation.
文摘A kinetic model was developed to describe the atom transfer radical polymerization (ATRP) of 2-(N,N-dimethylamino) ethyl methacrylate (DMAEMA). The model was based on a polymerization mechanism,which included the atom transfer equilibrium for primary radical, the propagation of growing polymer radical, and the atom transfer equilibrium for the growing polymer radical. An experiment was carried out to measure the conversion of monomer, the number-average molecular weight of polymer and molecular weight distribution for the ATRP process of DMAEMA. The experimental data were used to correlate the kinetic model and rate constants were obtained. The rate constants of activation and deactivation in the atom transfer equilibrium for primary radical are 1.0×10^4L·mol^-1·s^-1 and 0.04L·mol^-1·s^-1, respectively. The rate constant of the propagation of growing polymer radical is 8.50L·mol^-1·s^-1, and the rate constants of activation and deactivation in the atom transfer equilibrium for growing polymer radical are 0.045L·mol^-1·s^-1 and 1.2×10^5L·mol^-1·s^-1, respectively. The values of the rate constants represent the features of the ATRP process. The kinetic model was used to calculate the ATRP process of DMAEMA. The results show that the calculations agree well with the measurements.
基金Supported by the National Key R&D Program of China(2017YFB0602500)the Key Basic Research Items in Application Basic Research Program of Hebei Province,China(16964502D)
文摘Reactive dividing-wall column(RDWC) technology plays a critical role in the energy saving and high efficiency of chemical process.In this article, the process of co-producing ethyl acetate(EA) and n-butyl acetate(BA) with RDWC was studied.BA was not only the product, but also acted as entrainer to remove the water generated by the two esterification reactions.Experiments and simulations of the co-production process were carried out.It was found that the experimental results were in good agreement with the simulation results.Two kinds of RDWC structures(RDWC-FC and RDWC-RS) were proposed, and the co-production process operating parameters of the two types of RDWC were optimized by Aspen Plus respectively.The optimal operating parameters of the RDWC-FC were determined as follows: 0.6 of the reflux ratio of aqueous phase(RR), 0.66 of the vapor split(R_V) and 0.51 of the liquid split(R_L).And the optimal operating parameters of the RDWC-RS were shown as follows: RR was 0.295 and R_V was 0.61.Furthermore, the energy saving analysis of the co-production process was based on the annual output of 10000 tons of EA, compared with the traditional reaction distillation(RD) to prepare EA and BA, the reboiler duty of the RDWC-FC column could save 20.4%, TAC saving 23.6%; RDWC-RS reboiler energy consumption could save 17.0%, TAC 22.2%.
基金Funded by the National High-Tech Foundation(No. 2003 AA305920)
文摘2-Cetyl-3-20 keto acid(N-ethyl perfluorinated octyl sulfonamide) N-ethyl ester was synthesized by the reaction of N-ethyl-N-hydroxyethyl perfluorinated octyl sulfonamide and alky ketene dimer. The experimental results show that the yield of products can be 89% when the molar ratio of perfluorinated octyl sulfonamide to ketene dimer is 1 : 1.1 and the reaction lasts about four hours at 80 ℃. The structure of the product was characterized by FTIR and ^1HNMR. The product can dissolve in polar solvents such as NMP, DMAC, THF, DMSO, CHCl3, and 10% weight-loss temperature measured by TGA is 202℃.
基金the National Natural Science Foundation of China (No. 20672073) Shanghai Leading Academic Discipline Project (No. T0402)
文摘The title compound N-2-thiophenesulfonyl-a-L-phenylalanine ethyl ester has been synthesized. Complete assignments were achieved by IR, MS, ^1H NMR and single-crystal X-ray diffraction analyses. Using MTT assay, the inhibitory rate of the title compound on K562 cells (chronic myeloid leukemic cells) was measured and the result of preliminary bioassay showed that the title compound possesses antiproliferation effects on K562 cells. In order to investigate the relationship between structure and activity of the target compound, we report its crystal structure and biological behavior in the present paper. Crystallographic data: C15H17NO4S2, Mr = 339.42, monoclinic, space group P21, flack = -0.15(12), a = 5.7916(10), b = 11.5078(19), c = 12.924(2) A, β = 97.781(3)°, Z = 2, V = 853.4(2) A^3, De = 1.321 g/cm^3, F(000) = 356, -7≤h≤7, -10≤k≤14, -15 ≤ l≤15, R = 0.0628, wR = 0.1540 and μ(MoKa) = 0.327 mm^-1. The molecule comprises a benzene and a thiofuran rings, and the intramolecular N(1)-H(1A)…O(1) makes a five-membered ring of O(1)--C(6)-C(5)--N(1)--H(1A).
基金supported by the Fundamental Research Funds for the Central Universities(lzujbky-2010-137)Lanzhou Science and Technology Bureau Program Funds(2012-2-90)
文摘The title compound, N-(2-(1H-indol-3-yl)ethyl)-2-nitroaniline(C16H15N3O2, Mr = 281.31), has been synthesized by the multicomponent reaction of milder Ullmann, and its structure was characterized by 1H NMR, 13 C NMR, IR, H RMS(ESI) and single-crystal X-ray diffraction. It crystallizes in monoclinic, space group I2/c with a = 15.0212(10), b = 9.4911(6), c = 20.3075(13) A, β = 100.776(7)o, V = 2844.1(3)A3, Z = 8, Dc = 1.314 g/cm3, F(000) = 1184.0, μ = 0.089 mm-1, the final R = 0.0574 and w R = 0.1688 for 1701 observed reflections(I 】 2σ(I)). X-ray analysis indicates three major N(2)–H(2)···O(2), C(13)–H(13)···O(2), N(2)–H(2)···N(3) hydrogen bonds and π-π stacking interactions in the crystal structure. The preliminary biological test shows that the title compound has a good antitumor activity against A549 in vitro with the IC50 value of 35 μmol/L.
文摘When ethyl 3-fluoroalkyl-3-haloacrylate was treated with excess CH2N2,1-methyl-3-ethoxycarbonyl-4-fluoroalkylpyr azoles(3)and 1-methyl-5-ethoxycarbonyl-4-fluoroalkylpyrazoles(4)were obtained with a ratio of 90-95:10-5 in good yield.
文摘A nutritional fortifier N-(1-(phenylacetyl)-L-prolyl)glycine ethyl ester(4)was successfully synthesized through two synthetic schemes and characterized by IR,^1H-NMR,^13C-NMR,elemental analysis and X-ray single-crystal diffraction.The intermediate N-phenylacetyl-L-proline(2)was synthesized by the solid-liquid reaction of L-proline and phenylacetyl chloride directly.Compound 2(C13 H15 NO3,Mr=233.26)belongs to the orthorhombic system,space group P212121 with a=8.9468(3),b=9.3190(3),c=14.0453(4)A,V=1171.03(6)A^3,Z=4,Dc=1.323 g/cm^3,μ=0.773 mm^-1,F(000)=496.0,the final R=0.0313 and wR=0.0797 for all data.Compound 4(C17 H22 N2 O4,Mr=318.36)is of orthorhombic system,space group P212121 with a=6.5831(2),b=8.5536(2),c=28.9138(9)A,V=1628.11(8)A^3,Z=4,Dc=1.299 g/cm3,μ=0.763 mm-1,F(000)=680.0,the final R=0.0353 and wR=0.0816 for all data.
文摘Transgenic pigs have been produced with the aim of further improving pigs in terms of economic and environmental traits, but these animals have not been allowed to enter the food chain. As an alternative approach to generating pigs with novel traits of economic importance that cannot be introduced by conventional breeding, we propose a strategy for combining in vitro mutagenesis of pig primary cells with N-ethyl-N-nitrosourea (ENU) and somatic-cell nuclear transfer (SCNT) technology. To explore the feasibility of this strategy, we treated pig primary fibroblast cells with ENU, estimated the per-base mutation frequency induced by the mutagen, clonally cultured about 4000 of the mutagenized cells, and screened them for mutation within the coding region of the melanocortin-4 receptor (MC4R) gene, a key gene in energy homeostasis. Through this screening, we obtained 14 cell clones, each harboring a heterozygous base change within the coding region for MC4R. Of the mutant cell clones, each of two contained a mutant allele encoding MC4R with greatly reduced receptor activity. By SCNT using these cell clones as donors, pigs harboring mutated MC4R alleles with reduced receptor activity can be produced. Our strategy for generating pigs with novel genetic traits likely will be more acceptable to the public than is the use of transgenic technology.
基金Supported by the Jiangsu Natural Science Foundation (BK2008111,BK2010157)the National Natural Science Foundation of China (30770602)
文摘In this work,a calculation method of chemical kinetics was established for labeling reaction of 99mTc-N-ethyl-N2S2-memantine,a potential NMDA receptor imaging agent prepared in our laboratory.Four groups of vials (3 vials per group) were added with 0.02 mL (1 mg/mL) N-ethyl-N2S2Memantine,0.08 mL (40 mg/mL) GH,0.05 mL (10 mg/mL) EDTA-2Na,0.035 mL (2 mg/mL) SnF2,0.8 mL phosphate buffer(1mol/L,pH 6.5) and 37 MBq Na99mTcO4.The vials were incubated at 70℃,80℃,90℃ or 100℃.Samples were taken with capillary from the vials at 2,5,10,20,30,40 and 60min.Labeling yields were determined by TLC.Order of reaction n,rate constant k,activation energy Ea and half life t1/2 of labeling reaction were calculated with the kinetics software we compiled.Mean labeling yields of 99m Tc-N-ethyl-N2S2-memantine at 2,5,10,20,30,40 and 60min were (1) 13.5,15.7,34.0,64.8,81.9,91.4 and 95.4 at 70℃;(2) 13.2,20.5,40.1,70.0,88.2,94.5 and 95.6 at 80℃;(3) 15.6,22.9,43.7,74.3,87.2,93.4 and 96.1 at 90℃;and (4) 20.5,25.8,45.3,81.1,92.2,95.6 and 96.0 at 100℃.The other parameters were;n =1;k=0.053,0.061,0.063 and 0.076 L/min at 70℃,80℃,90℃ and 100℃,respectively;Ea=12.38 kJ/L;t1/2=13.11,11.45,11.05 and 9.07min at 70℃,80℃,90℃ and 100℃,respectively.The mean labeling yield increased with temperature and time,optimized at 100℃ and 40-60min.The concentration of 99mTc-N-ethyl-N2S2-Memantine was larger than that of Na99mTcO4,so n=1.The k increased with reaction,hence the accelerated reaction rate at higher temperatures.The labeling reaction was not so difficult because of the low Ea.The t1/2 decreased with increasing reaction temperature,hence the acceleration of labeling reaction.