2,3-Bis(hydroxymethyl)-2,3-dinitro-1,4-butanediol(C6H12N2O8) was synthesized by condensation,cyclization,oxidative dimerization and deketalization of nitromethane with a total yield of 42.4%.The structure of the t...2,3-Bis(hydroxymethyl)-2,3-dinitro-1,4-butanediol(C6H12N2O8) was synthesized by condensation,cyclization,oxidative dimerization and deketalization of nitromethane with a total yield of 42.4%.The structure of the title compound was characterized by 1H NMR,13C NMR,FT-IR,elementary analysis,and X-ray single-crystal diffraction analysis,which reveals that the title compound crystallizes in triclinic,space group P with a = 0.6324(2),b = 0.6454(3),c = 0.7062(3) nm,α= 111.550(4),β= 95.505(4),γ= 113.395(4)°,V = 0.23595(16) nm3,Z = 1,Mr = 240.18,Dc = 1.690 g·cm-3,μ = 0.159 mm-1,F(000) = 126,R = 0.0304 and wR = 0.0907.展开更多
We report here a solid-phase synthesis of 1, 4-disubstituted 1, 2, 3-triazole using polystyrene-supported selenium resin. The resin used here not only works as a simple linker, but also assists the crucial α-alkylati...We report here a solid-phase synthesis of 1, 4-disubstituted 1, 2, 3-triazole using polystyrene-supported selenium resin. The resin used here not only works as a simple linker, but also assists the crucial α-alkylation reaction and selenoxide syn-elimimation, which ensures the purity of the products.展开更多
An efficient and easy method for one-pot three-component synthesis of l,3-disubstituted-3H-benzo[f]chromenes by the condensation of naphtol,aromatic aldehyde derivatives and phenylacetylene in the presence of ferric h...An efficient and easy method for one-pot three-component synthesis of l,3-disubstituted-3H-benzo[f]chromenes by the condensation of naphtol,aromatic aldehyde derivatives and phenylacetylene in the presence of ferric hydrogensulfate[Fe(HSO4)3], has been described.The catalyst displayed high activity which afforded the corresponding 1,3-disubstituted-3H-benzo[f]chromenes in satisfying yields.Alkyl-substituted phenols were examined and the corresponding benzopyran derivatives were synthesized in moderate yields.Heterogeneous nature of the using catalyst made it reusable for further chemical reactions.展开更多
Two new 1,3-oxazin derivatives, C22H24N2O5 (3I) and C19H16N2O5(3II), have been synthesized via an unusual cascade reaction. The attractive aspect of this cascade reaction is that the novel construction of 1,3-oxaz...Two new 1,3-oxazin derivatives, C22H24N2O5 (3I) and C19H16N2O5(3II), have been synthesized via an unusual cascade reaction. The attractive aspect of this cascade reaction is that the novel construction of 1,3-oxazine and the direct C-N bond formation from C-C bond can be easily achieved via pyridine-mediated acylation in a one-pot operation. Both compounds have been synthesized and characterized by elemental analysis, IR, NMR spectra and X-ray single-crystal diffraction. Compound 3I crystallizes in monoclinic, space group P21/n with α = 16.282(4), b = 7.4117(18), c = 17.256(5) A, β = 103.193(9)°, V = 2027.4(9) A3, Mr = 396.43, Z = 4, Dc= 1.299 g/cm3, F(000) = 840, MoKa radiation (λ = 0.71073 A), the final R = 0.0771 and wR = 0.1582 for 3662 were observed reflections with I 〉 2σ(I). Compound 3II crystallizes in triclinic, space group Pī with α = 7.1265(9), b = 10.1071(13), c = 23.529(3) A, α = 97.463(9), β = 96.981(9), γ = 94.345(9)°, V = 1600.5(4) A3, Z = 4, Dc = 1.409 g/cm3, F(000) = 736, CuKa radiation (λ = 1.54186 A), the final R = 0.0515 and wR = 0.1241 for 4920 observed reflections with I 〉 2σ(I). The preliminary antibacterial activities of 2 and 3 against E. coli and S. aureuswere investigated. The results showed that the inhibiting effect of 3 was higher than that of 2.展开更多
The title compound, 4-tert-butyl-6-(4-chlorophenyl)-3,6-dihydro-2H-1,3-thiazin- 2-iminium chloride (C14H18C12N2S), has been synthesized by the reaction of 1-(4-chlorophenyl)- 4,4-dimethylpent-1-en-3-one with thi...The title compound, 4-tert-butyl-6-(4-chlorophenyl)-3,6-dihydro-2H-1,3-thiazin- 2-iminium chloride (C14H18C12N2S), has been synthesized by the reaction of 1-(4-chlorophenyl)- 4,4-dimethylpent-1-en-3-one with thiourea, and its crystal structure was determined by single- crystal X-ray diffraction. The crystal belongs to the monoclinic system, space group P211c with a = 16.3064(11), b = 9.4471(6), c = 11.2626 (8)A, β = 108.400(1)°, Z = 4, V = 1646.28(19) A^3, Mr = 317.26, Dc = 1.280 g/cm^3, S = 1.078,μ = 0.510 mm^-1, F(000) = 664, the final R = 0.0514 and wR = 0.1412 for 3210 observed reflections (I 〉 2σ(I)). The thiazine ring system displays a twisted boat conformation, and three N-H,..Cl hydrogen bonds exist in the crystal. The combination of two N-H...Cl hydrogen bonds generate an R2^1 (6) ring.展开更多
The crystal structure of the new cinnamide derivative(E)-1-(4-(4-chlorobenzyl)piperazin-1-yl)-3-(benzo[d][1,3]dioxol-5-yl)prop-2-en-1-one(C(21)H(21)ClN2O3, Mr = 384.85) was determined by single-crystal X...The crystal structure of the new cinnamide derivative(E)-1-(4-(4-chlorobenzyl)piperazin-1-yl)-3-(benzo[d][1,3]dioxol-5-yl)prop-2-en-1-one(C(21)H(21)ClN2O3, Mr = 384.85) was determined by single-crystal X-ray diffraction method. Compound 5 crystallizes in the monoclinic system, space group P21/c with a = 11.762(2), b = 15.279(3), c = 11.865(2) , β = 116.57(3)°, V = 1907.1(7) 3, Z = 4, Dc = 1.340 g/cm3, F(000) = 808, μ = 0.224 mm-1, Mo Kα radiation(λ = 0.71073 ), the final R = 0.0565 and w R = 0.1479 for 2318 observed reflections with I 〉 2σ(I). Intramolecular C(9)–H(9A)···O(1) interactions as well as intermolecular C(16)–H(16A)···O(1) hydrogen bonds help to stabilize the crystal structure. The bioassay results indicated that the title compound displayed promising neuroprotection in vitro and in vivo, and suppressed apoptosis of glutamate-induced PC12 cells.展开更多
The title compound 3,9-bis(pyridin-2-yl)-2,4,8,10-tetraoxaspiro[5.5]undecane 4(C17H18N2O4) has been synthesized by the reaction of 2,2-bis(hydroxymethyl)propane-1,3-diol with pyridine-2-carbaldehyde in the prese...The title compound 3,9-bis(pyridin-2-yl)-2,4,8,10-tetraoxaspiro[5.5]undecane 4(C17H18N2O4) has been synthesized by the reaction of 2,2-bis(hydroxymethyl)propane-1,3-diol with pyridine-2-carbaldehyde in the presence of p-toluenesulfonic acid,and characterized by IR,1H-NMR and X-ray single-crystal diffraction.The crystal belongs to monoclinic system,space group C2/c with a = 25.133(2),b = 5.7219(5),c = 21.942(2)(A°) ,β = 99.145(2)°,V = 3115.3(5)(A°)^3,Z = 8,Dc = 1.340 g/cm^3,Mr = 314.33,F(000) = 1328,μ = 0.097 mm-1,MoKa radiation(λ = 0.71073),R = 0.0352 and wR = 0.1022 for 2486 observed reflections with I 〉 2σ(I).X-ray analysis reveals that the two 1,3-dioxane rings passing through the central spiro-C atom both adopt chair conformation.Intermolecular C-H…π,C-H…O and C-H…N weak interactions link the molecules to form a three-dimensional samdwich,which are effective in the stabilization of the crystal structure.展开更多
The synthetic process for 2,2-dimethyl-5-nitro-5-nitroso-1,3-dioxane(DMNNDO) was improved by using tri(hydroxymethyl)nitromethane and acetone as starting materials through a "one-pot" method combined with alkali...The synthetic process for 2,2-dimethyl-5-nitro-5-nitroso-1,3-dioxane(DMNNDO) was improved by using tri(hydroxymethyl)nitromethane and acetone as starting materials through a "one-pot" method combined with alkaline hydrolysis and nitrosation reactions. The yield of DMNNDO was increased from 37% to 45%. The structure of DMNNDO was characterized by IR,^1H NMR,^13 C NMR,and elemental analysis. Also the thermal decomposition of DMNNDO was studied by using DSC and TG-DTG to find that there are primarily two exothermic decomposition processes between 90 and 300 oC. The crystal structure of DMNNDO was studied by X-ray single-crystal diffraction for the first time. The molecular structure exists as a dimeric form due to the presence of nitroso group. The crystal belongs to monoclinic system,space group C2/c with a = 14.515(3),b = 9.955(2),c = 11.897(2) °,β = 98.500(3)°,V = 1.6998(2) nm^3,Z = 8,D_c = 1.486 g×cm^-3,μ = 0.128 mm^-1,F(000) = 800,S = 1.055,R = 0.0358 and wR = 0.0917. In particular,DMNNDO could be easily hydrolyzed in hydrous systems and the hydrolysis mechanism in CDCl_3 was revealed by means of NMR monitoring.展开更多
The synthesis of T_8, T_ 10 and T_ 12 silsesquioxane cages from a range of starting materials: phenyl-cis-tetrol, 1,3-divinyltetraethoxydisiloxane and cyclopentyl T resins by using tetra n-butylammonium fluoride(TBA...The synthesis of T_8, T_ 10 and T_ 12 silsesquioxane cages from a range of starting materials: phenyl-cis-tetrol, 1,3-divinyltetraethoxydisiloxane and cyclopentyl T resins by using tetra n-butylammonium fluoride(TBAF) as the catalyst is described in this paper. The reaction yields obtained viathe current route are better compared to those viathe literature routes. Some of the cage compounds have been characterized by X-ray crystallography.展开更多
A total synthesis of (E,E)-3,7-dimethyl-2,6-decadiene-1,10-diol, using 1,3-transformation of 2, 3-epoxy alcohol and Claisen rearrangement of allyl vinyl ether as key steps, is described.
The title compound, N,N'-bis-[3-chloro-5-S-(l-menthyloxy)-2(5H)-4-furanon-yl]- propane-l,3-diamine (C31H48Cl2N2O6, Mr = 615.61), has been synthesized and characterized by IR, 1H NMR, MS, elemental analysis and ...The title compound, N,N'-bis-[3-chloro-5-S-(l-menthyloxy)-2(5H)-4-furanon-yl]- propane-l,3-diamine (C31H48Cl2N2O6, Mr = 615.61), has been synthesized and characterized by IR, 1H NMR, MS, elemental analysis and single-crystal X-ray diffraction. The crystal crystallizes in the monoclinic system, space group C2 with a = 16.1091(4), b = 11.1880(3), c = 19.2854(5) A, β = 106.297(2)°, V = 3336.12(15) A3, Z = 4, Dc = 1.226 mg/m3,μ = 0.237 mm^-1, F(000) = 1320, the final R = 0.0531 and wR = 0.0700 for 2760 observed reflections (I 〉 2σ(I)). X-ray analysis reveals that the title compound possesses four rings: two chiral five-membered furanone rings and two six-membered cyclohexane rings with chair conformation, containing eight chiral centers: C2(S), C3(R), C5(R), C10(S), C18(S), C21(R), C22(S) and C25(R). The structure is stabilized by N-H…O hydrogen bonding interaction.展开更多
A new copper(II) complex 3, Cu(C17H13F3O3)2·C5H5N, has been synthesized and characterized by single-crystal X-ray diffraction. It crystallizes in monoclinic, space group C2/c with a = 17.8511(7), b = 17.413...A new copper(II) complex 3, Cu(C17H13F3O3)2·C5H5N, has been synthesized and characterized by single-crystal X-ray diffraction. It crystallizes in monoclinic, space group C2/c with a = 17.8511(7), b = 17.4136(7), c = 13.9425(7) A, β = 124.4830(10)°, V = 3572.5(3) A^3, Z = 4, C39H29CuF6NO6, Mr = 785.17,/7(000) = 1604, T = 292(2) K, Dc = 1.460 g/cm^3 and p = 0.691 mm^-1. The structure was refined to R = 0.0477 and wR = 0.1110 for 2935 observed reflections with I 〉 2σ(I). For the title compound, X-ray analysis reveals that the copper(II) is penta-coordinated by four oxygen atoms from the corresponding 1-(4-(benzyloxy)phenyl)-4,4,4-trifluorobutane-1,3-dione ligands and one nitrogen atom of pyridine, forming a distorted square pyramidal geometry. It is found that the trifluoromethyl group, F(1)/F(1'), F(2)/F(2') and F(3)/F(3')), is disordered over two orientations in an approximate 3:1 ratio.展开更多
A facile synthesis of the analog of curcumin. 1,7-bis (4-hydroxyphenyl)-3-hydroxy-1.3-heptadien-5-one 1 was achieved. The key step was completed through the regioselective condensation of ketone 5 and acyl chloride 7.
The key intermediate, 2-isopropyl-2-(3-methyl-1-benzoxyl-5-phenylsulfonyl-3E-pentenyl)-1, 3-dithiocycllohexane(Ⅲ), for the total synthesis of Sarcophytol-A (1)was prepared through 7 steps from acetone. The key steps ...The key intermediate, 2-isopropyl-2-(3-methyl-1-benzoxyl-5-phenylsulfonyl-3E-pentenyl)-1, 3-dithiocycllohexane(Ⅲ), for the total synthesis of Sarcophytol-A (1)was prepared through 7 steps from acetone. The key steps are nucleophilic addition of 2-1ithio-2-isopropyl-1,3-dithiocyclohexane to aldehyde 5 and double bond migration reaction of allylic alcohol 9 and 10.展开更多
The title compound tert-butyl 4-[(E)-4-(1,3-dioxo-1,3-dihydro-2H-isoindol-2-yl)- 1-butenyl] benzoate has been synthesized and characterized by X-ray crystallography. It crystallizes in monoclinic, space group C2/c...The title compound tert-butyl 4-[(E)-4-(1,3-dioxo-1,3-dihydro-2H-isoindol-2-yl)- 1-butenyl] benzoate has been synthesized and characterized by X-ray crystallography. It crystallizes in monoclinic, space group C2/c with a = 14.875(3), b = 8.9796(13), c = 34.736(6) A°, β = 95.981(4)°, V= 4614.4(14)A°^3, Z= 8, Dc = 1.213 g/cm^3, F(000) = 1792,μ(MoKα) = 0.084 mm^-1, R = 0.0602 and wR = 0.1445 for 4613 unique reflections with 2272 observed ones (I〉 2σ(I)). The results of crystal structure determination show that the title compound has a layer structure, and the two benzene rings in molecule are parallel to each other.展开更多
The synthesis of the title molecule was achieved by the reaction of 2,4-dichloro- benzoyl chloride with potassium thiocyanate in 1:1 molar ratio in dry acetonitrile to afford the corresponding isothiocyante in situ f...The synthesis of the title molecule was achieved by the reaction of 2,4-dichloro- benzoyl chloride with potassium thiocyanate in 1:1 molar ratio in dry acetonitrile to afford the corresponding isothiocyante in situ followed by the treatment with 2-aminobiphenyl. The structure of the target compound was established by elemental analysis, FTIR, 1H, 13C NMR and mass spectroscopy and unequivocally confirmed by the crystallographic data. The title compound crystallizes in the monoclinic space group P21/n with a = 13.356(2), b = 7.0761(11), c = 20.539(3) A, β = 105.723(4)°, V= 1868.5(5) A3 and Z = 4.展开更多
The title compound (C40H42N2) has been synthesized by the reaction of l-(l- naphthyl)-l-phenyl-3-chloropropylene and bis(4-(diethylamino) phenyl)methanone, and characterized by IR, ^1H NMR, MS and X-ray diffra...The title compound (C40H42N2) has been synthesized by the reaction of l-(l- naphthyl)-l-phenyl-3-chloropropylene and bis(4-(diethylamino) phenyl)methanone, and characterized by IR, ^1H NMR, MS and X-ray diffraction analysis. The crystal belongs to the monoclinic system, space group P21/c with a = 17.047(3), b = 10.807(2), c = 18.494(4) A, β = 105.727(4)°, V= 3279.4(11) A^3, Mr = 550.76, Z = 4, Dc = 1.115 g/cm^3,μ(MoKa) = 0.085 mm^-1, F(000) = 1184, the final R = 0.0625 and wR = 0.1384 for 2276 observed reflections (1 〉 2σ(I)). X-ray analysis reveals that the butadiene fragment adopts a planar cisiod conformation and makes a dihedral angel of 69.4(2)° with the naphthalene ring.展开更多
New structural phospholipids 1.3-cyclic monoalkyl(acyl)-rac-glycerothiophosphates of uridine were synthesized. The strategy for the synthesis is using hexaethylphosphorous triamide, activated by a catalytic amount of ...New structural phospholipids 1.3-cyclic monoalkyl(acyl)-rac-glycerothiophosphates of uridine were synthesized. The strategy for the synthesis is using hexaethylphosphorous triamide, activated by a catalytic amount of iodine, as the phosphorylating reagent. Their structures were confirmed by (1)HNMR, (31)PNMR, IR and elemental analysis.展开更多
基金Supported by the National "973" project (No. 613740102)
文摘2,3-Bis(hydroxymethyl)-2,3-dinitro-1,4-butanediol(C6H12N2O8) was synthesized by condensation,cyclization,oxidative dimerization and deketalization of nitromethane with a total yield of 42.4%.The structure of the title compound was characterized by 1H NMR,13C NMR,FT-IR,elementary analysis,and X-ray single-crystal diffraction analysis,which reveals that the title compound crystallizes in triclinic,space group P with a = 0.6324(2),b = 0.6454(3),c = 0.7062(3) nm,α= 111.550(4),β= 95.505(4),γ= 113.395(4)°,V = 0.23595(16) nm3,Z = 1,Mr = 240.18,Dc = 1.690 g·cm-3,μ = 0.159 mm-1,F(000) = 126,R = 0.0304 and wR = 0.0907.
基金the National Natural Science Foundation of China(No.20332060)the Natural Science Foundation of Zhejiang Province(No.Y405407).
文摘We report here a solid-phase synthesis of 1, 4-disubstituted 1, 2, 3-triazole using polystyrene-supported selenium resin. The resin used here not only works as a simple linker, but also assists the crucial α-alkylation reaction and selenoxide syn-elimimation, which ensures the purity of the products.
文摘An efficient and easy method for one-pot three-component synthesis of l,3-disubstituted-3H-benzo[f]chromenes by the condensation of naphtol,aromatic aldehyde derivatives and phenylacetylene in the presence of ferric hydrogensulfate[Fe(HSO4)3], has been described.The catalyst displayed high activity which afforded the corresponding 1,3-disubstituted-3H-benzo[f]chromenes in satisfying yields.Alkyl-substituted phenols were examined and the corresponding benzopyran derivatives were synthesized in moderate yields.Heterogeneous nature of the using catalyst made it reusable for further chemical reactions.
基金supported by the National Natural Science Foundation of China(No.81071144)Natural Science Foundation of Guangdong Province(No.9451806001002961)
文摘Two new 1,3-oxazin derivatives, C22H24N2O5 (3I) and C19H16N2O5(3II), have been synthesized via an unusual cascade reaction. The attractive aspect of this cascade reaction is that the novel construction of 1,3-oxazine and the direct C-N bond formation from C-C bond can be easily achieved via pyridine-mediated acylation in a one-pot operation. Both compounds have been synthesized and characterized by elemental analysis, IR, NMR spectra and X-ray single-crystal diffraction. Compound 3I crystallizes in monoclinic, space group P21/n with α = 16.282(4), b = 7.4117(18), c = 17.256(5) A, β = 103.193(9)°, V = 2027.4(9) A3, Mr = 396.43, Z = 4, Dc= 1.299 g/cm3, F(000) = 840, MoKa radiation (λ = 0.71073 A), the final R = 0.0771 and wR = 0.1582 for 3662 were observed reflections with I 〉 2σ(I). Compound 3II crystallizes in triclinic, space group Pī with α = 7.1265(9), b = 10.1071(13), c = 23.529(3) A, α = 97.463(9), β = 96.981(9), γ = 94.345(9)°, V = 1600.5(4) A3, Z = 4, Dc = 1.409 g/cm3, F(000) = 736, CuKa radiation (λ = 1.54186 A), the final R = 0.0515 and wR = 0.1241 for 4920 observed reflections with I 〉 2σ(I). The preliminary antibacterial activities of 2 and 3 against E. coli and S. aureuswere investigated. The results showed that the inhibiting effect of 3 was higher than that of 2.
基金supported by the National Project of Scientific and Technical Supporting Programs Funded by Ministry of Science & Technology of China (No 2006BAE01A01-4)
文摘The title compound, 4-tert-butyl-6-(4-chlorophenyl)-3,6-dihydro-2H-1,3-thiazin- 2-iminium chloride (C14H18C12N2S), has been synthesized by the reaction of 1-(4-chlorophenyl)- 4,4-dimethylpent-1-en-3-one with thiourea, and its crystal structure was determined by single- crystal X-ray diffraction. The crystal belongs to the monoclinic system, space group P211c with a = 16.3064(11), b = 9.4471(6), c = 11.2626 (8)A, β = 108.400(1)°, Z = 4, V = 1646.28(19) A^3, Mr = 317.26, Dc = 1.280 g/cm^3, S = 1.078,μ = 0.510 mm^-1, F(000) = 664, the final R = 0.0514 and wR = 0.1412 for 3210 observed reflections (I 〉 2σ(I)). The thiazine ring system displays a twisted boat conformation, and three N-H,..Cl hydrogen bonds exist in the crystal. The combination of two N-H...Cl hydrogen bonds generate an R2^1 (6) ring.
基金Supported by the National Natural Science Foundation of China(No.81371451)the Natural Science Foundation of Jiangsu Province(No.BK20131390)
文摘The crystal structure of the new cinnamide derivative(E)-1-(4-(4-chlorobenzyl)piperazin-1-yl)-3-(benzo[d][1,3]dioxol-5-yl)prop-2-en-1-one(C(21)H(21)ClN2O3, Mr = 384.85) was determined by single-crystal X-ray diffraction method. Compound 5 crystallizes in the monoclinic system, space group P21/c with a = 11.762(2), b = 15.279(3), c = 11.865(2) , β = 116.57(3)°, V = 1907.1(7) 3, Z = 4, Dc = 1.340 g/cm3, F(000) = 808, μ = 0.224 mm-1, Mo Kα radiation(λ = 0.71073 ), the final R = 0.0565 and w R = 0.1479 for 2318 observed reflections with I 〉 2σ(I). Intramolecular C(9)–H(9A)···O(1) interactions as well as intermolecular C(16)–H(16A)···O(1) hydrogen bonds help to stabilize the crystal structure. The bioassay results indicated that the title compound displayed promising neuroprotection in vitro and in vivo, and suppressed apoptosis of glutamate-induced PC12 cells.
基金supported by the National Natural Science Foundation of China (No. 20872051 and 21002009)the Scientific and Technological Project of Changzhou (CJ20115019)the Priority Academic Program Development of Jiangsu Higher Education Institutions
文摘The title compound 3,9-bis(pyridin-2-yl)-2,4,8,10-tetraoxaspiro[5.5]undecane 4(C17H18N2O4) has been synthesized by the reaction of 2,2-bis(hydroxymethyl)propane-1,3-diol with pyridine-2-carbaldehyde in the presence of p-toluenesulfonic acid,and characterized by IR,1H-NMR and X-ray single-crystal diffraction.The crystal belongs to monoclinic system,space group C2/c with a = 25.133(2),b = 5.7219(5),c = 21.942(2)(A°) ,β = 99.145(2)°,V = 3115.3(5)(A°)^3,Z = 8,Dc = 1.340 g/cm^3,Mr = 314.33,F(000) = 1328,μ = 0.097 mm-1,MoKa radiation(λ = 0.71073),R = 0.0352 and wR = 0.1022 for 2486 observed reflections with I 〉 2σ(I).X-ray analysis reveals that the two 1,3-dioxane rings passing through the central spiro-C atom both adopt chair conformation.Intermolecular C-H…π,C-H…O and C-H…N weak interactions link the molecules to form a three-dimensional samdwich,which are effective in the stabilization of the crystal structure.
文摘The synthetic process for 2,2-dimethyl-5-nitro-5-nitroso-1,3-dioxane(DMNNDO) was improved by using tri(hydroxymethyl)nitromethane and acetone as starting materials through a "one-pot" method combined with alkaline hydrolysis and nitrosation reactions. The yield of DMNNDO was increased from 37% to 45%. The structure of DMNNDO was characterized by IR,^1H NMR,^13 C NMR,and elemental analysis. Also the thermal decomposition of DMNNDO was studied by using DSC and TG-DTG to find that there are primarily two exothermic decomposition processes between 90 and 300 oC. The crystal structure of DMNNDO was studied by X-ray single-crystal diffraction for the first time. The molecular structure exists as a dimeric form due to the presence of nitroso group. The crystal belongs to monoclinic system,space group C2/c with a = 14.515(3),b = 9.955(2),c = 11.897(2) °,β = 98.500(3)°,V = 1.6998(2) nm^3,Z = 8,D_c = 1.486 g×cm^-3,μ = 0.128 mm^-1,F(000) = 800,S = 1.055,R = 0.0358 and wR = 0.0917. In particular,DMNNDO could be easily hydrolyzed in hydrous systems and the hydrolysis mechanism in CDCl_3 was revealed by means of NMR monitoring.
文摘The synthesis of T_8, T_ 10 and T_ 12 silsesquioxane cages from a range of starting materials: phenyl-cis-tetrol, 1,3-divinyltetraethoxydisiloxane and cyclopentyl T resins by using tetra n-butylammonium fluoride(TBAF) as the catalyst is described in this paper. The reaction yields obtained viathe current route are better compared to those viathe literature routes. Some of the cage compounds have been characterized by X-ray crystallography.
文摘A total synthesis of (E,E)-3,7-dimethyl-2,6-decadiene-1,10-diol, using 1,3-transformation of 2, 3-epoxy alcohol and Claisen rearrangement of allyl vinyl ether as key steps, is described.
基金Supported by the National Natural Science Foundation of China (No. 20772035)the Natural Science Foundation of Guangdong Province (No. 5300082)
文摘The title compound, N,N'-bis-[3-chloro-5-S-(l-menthyloxy)-2(5H)-4-furanon-yl]- propane-l,3-diamine (C31H48Cl2N2O6, Mr = 615.61), has been synthesized and characterized by IR, 1H NMR, MS, elemental analysis and single-crystal X-ray diffraction. The crystal crystallizes in the monoclinic system, space group C2 with a = 16.1091(4), b = 11.1880(3), c = 19.2854(5) A, β = 106.297(2)°, V = 3336.12(15) A3, Z = 4, Dc = 1.226 mg/m3,μ = 0.237 mm^-1, F(000) = 1320, the final R = 0.0531 and wR = 0.0700 for 2760 observed reflections (I 〉 2σ(I)). X-ray analysis reveals that the title compound possesses four rings: two chiral five-membered furanone rings and two six-membered cyclohexane rings with chair conformation, containing eight chiral centers: C2(S), C3(R), C5(R), C10(S), C18(S), C21(R), C22(S) and C25(R). The structure is stabilized by N-H…O hydrogen bonding interaction.
基金supported by the Natural Science Foundation of the Educational Commission of Hubei Province (No. Q20082202)
文摘A new copper(II) complex 3, Cu(C17H13F3O3)2·C5H5N, has been synthesized and characterized by single-crystal X-ray diffraction. It crystallizes in monoclinic, space group C2/c with a = 17.8511(7), b = 17.4136(7), c = 13.9425(7) A, β = 124.4830(10)°, V = 3572.5(3) A^3, Z = 4, C39H29CuF6NO6, Mr = 785.17,/7(000) = 1604, T = 292(2) K, Dc = 1.460 g/cm^3 and p = 0.691 mm^-1. The structure was refined to R = 0.0477 and wR = 0.1110 for 2935 observed reflections with I 〉 2σ(I). For the title compound, X-ray analysis reveals that the copper(II) is penta-coordinated by four oxygen atoms from the corresponding 1-(4-(benzyloxy)phenyl)-4,4,4-trifluorobutane-1,3-dione ligands and one nitrogen atom of pyridine, forming a distorted square pyramidal geometry. It is found that the trifluoromethyl group, F(1)/F(1'), F(2)/F(2') and F(3)/F(3')), is disordered over two orientations in an approximate 3:1 ratio.
文摘A facile synthesis of the analog of curcumin. 1,7-bis (4-hydroxyphenyl)-3-hydroxy-1.3-heptadien-5-one 1 was achieved. The key step was completed through the regioselective condensation of ketone 5 and acyl chloride 7.
基金Supported by the National Natural Science Foundation of China State Educational Commission Foundation of China
文摘The key intermediate, 2-isopropyl-2-(3-methyl-1-benzoxyl-5-phenylsulfonyl-3E-pentenyl)-1, 3-dithiocycllohexane(Ⅲ), for the total synthesis of Sarcophytol-A (1)was prepared through 7 steps from acetone. The key steps are nucleophilic addition of 2-1ithio-2-isopropyl-1,3-dithiocyclohexane to aldehyde 5 and double bond migration reaction of allylic alcohol 9 and 10.
文摘The title compound tert-butyl 4-[(E)-4-(1,3-dioxo-1,3-dihydro-2H-isoindol-2-yl)- 1-butenyl] benzoate has been synthesized and characterized by X-ray crystallography. It crystallizes in monoclinic, space group C2/c with a = 14.875(3), b = 8.9796(13), c = 34.736(6) A°, β = 95.981(4)°, V= 4614.4(14)A°^3, Z= 8, Dc = 1.213 g/cm^3, F(000) = 1792,μ(MoKα) = 0.084 mm^-1, R = 0.0602 and wR = 0.1445 for 4613 unique reflections with 2272 observed ones (I〉 2σ(I)). The results of crystal structure determination show that the title compound has a layer structure, and the two benzene rings in molecule are parallel to each other.
文摘The synthesis of the title molecule was achieved by the reaction of 2,4-dichloro- benzoyl chloride with potassium thiocyanate in 1:1 molar ratio in dry acetonitrile to afford the corresponding isothiocyante in situ followed by the treatment with 2-aminobiphenyl. The structure of the target compound was established by elemental analysis, FTIR, 1H, 13C NMR and mass spectroscopy and unequivocally confirmed by the crystallographic data. The title compound crystallizes in the monoclinic space group P21/n with a = 13.356(2), b = 7.0761(11), c = 20.539(3) A, β = 105.723(4)°, V= 1868.5(5) A3 and Z = 4.
基金The project was supported by the National 863 Program of China (No. 2002AA325050)
文摘The title compound (C40H42N2) has been synthesized by the reaction of l-(l- naphthyl)-l-phenyl-3-chloropropylene and bis(4-(diethylamino) phenyl)methanone, and characterized by IR, ^1H NMR, MS and X-ray diffraction analysis. The crystal belongs to the monoclinic system, space group P21/c with a = 17.047(3), b = 10.807(2), c = 18.494(4) A, β = 105.727(4)°, V= 3279.4(11) A^3, Mr = 550.76, Z = 4, Dc = 1.115 g/cm^3,μ(MoKa) = 0.085 mm^-1, F(000) = 1184, the final R = 0.0625 and wR = 0.1384 for 2276 observed reflections (1 〉 2σ(I)). X-ray analysis reveals that the butadiene fragment adopts a planar cisiod conformation and makes a dihedral angel of 69.4(2)° with the naphthalene ring.
文摘New structural phospholipids 1.3-cyclic monoalkyl(acyl)-rac-glycerothiophosphates of uridine were synthesized. The strategy for the synthesis is using hexaethylphosphorous triamide, activated by a catalytic amount of iodine, as the phosphorylating reagent. Their structures were confirmed by (1)HNMR, (31)PNMR, IR and elemental analysis.