Synthesis and Antitumor Activity of 3-[2-(4-Hydroxy-Phenyl)-Ethyl]-Benzo[d] Isoxazole-4,6-Diol

A new phloretin derivative 1 3-[2-(4-hydroxy-phenyl)-ethyl]-benzo[d] isoxazole-4,6-diol (yield 63%) was synthesized from phloretin by carbonyl nucleophilic addition condensation reaction. Its structure was characterized by 1H NMR, 13C NMR and HR-MS. The phloretin, compound 1, resveratrol and acetylated resveratrol were determined by comparing them with paclitaxel. Anti-tumor activity of alcohol on SPC-A1, EC109, A549, MCF-7 and MDA-MB-231 cell lines. Compound 1 showed better antitumor activity than docetaxel against A549 tumor cells.

Preparation of Ni(HCO_3)_2 and its catalytic performance in synthesis of benzoin ethyl ether

Ni（HCO3）2 with unique phase and high crystallinity was synthesized with urea hydrolysis. The as-prepared samples were well characterized in detail. N2 adsorption and desorption result manifests a high surface area of 99.03 m2/g with a pore size of 7.8 nm. Scanning electron microscopy （SEM） and particle size distribution reveal that the diameters of the formed pellets are uniform. Thermogravimetry （TG） analysis result shows that 500 ℃ could be the appropriate temperature for converting Ni（HCO3）2 precursors into NiO via a thermal decomposition process. CO2 and NH3 temperature-programmed desorption results show that Ni（HCO3）2 has explicit acid-base sites. Transmission electron microscopy （TEM） results vividly indicate that the pellets are aggregated by hexagonal platelets and possess porous structures. Ni（HCO3）2 can efficiently catalyze the one-step synthesis of benzoin ethyl ether from benzaldehyde and ethanol, with the conversion ofbenzaldehyde up to 57.5% and nearly 100% selectivity of benzoin ethyl ether.

Synthesis and Purification of Porphyrin-Schiff Base Using Ethyl Vanillin

A novel porphyrin-Schiff base was synthesized via the condensation of 5-（4-aminophenyl） -10,15,20-triphenylperphyrin and ethyl vanillin. After analyzing the level of purification of the perphyrin-Schiff base, it was successfully separated. This perphyrin-Schiff base was characterized by using UV-Vis, IR,^1H NMR and MS spectroscopy.

Synthesis and in vitro-Anti-hepatitis B Virus Activities of Several Ethyl 5-Hydroxy-1H-indole-3-carboxylates

A series of ethyl 5-hydroxyindole-3-earboxylates 6a-10r was designed and synthesized. The structures of all the compounds were confirmed by IR, ^1H NMR, and MS and their anti-hepatitis B virus （HBV） activities were evaluated in 2.2.15 cells. Among them, compound 7g { ethyl 5-hydroxy-2- [ （ 3-methoxyphenylsulfinyl ） methyl ] -1-methyl-4- [ （4-methylpiperazin-1-yl） methyl ]-1H-indole-3-carboxylate} displays a significant anti-HBV activity, which is more potent than the positive control lamivudine.

Synthesis and biological evaluation of ethyl 6-alkoxy-7-phenyl-4-hydroxy-3-quinolinecarboxylates against Eimeria tenella

A series of ethyl 6-alkoxy-7-phenyl-4-hydroxy-3-quinolinecarboxylates were designed and synthesized.Their structures were confirmed by ~1H NMR,^(13)C NMR,IR and HRMS.The biological activities were primarily evaluated against Eimeria tenella according to Anticoccidial Index(ACI) method in vivo.The results showed that compounds 5e,5f and 5i exhibited anticoccidial activities against E.tenella at 27 mg kg^(-1).

Synthesis of 7-Ethyl-10-hydroxycamptothecin and Proposed Reaction Mechanism

The improved 3 step preparation of a key antitumor agent, 7 ethyl 10 hydroxycamptothecin(SN 38), which consists of ethylation, oxidation and photo chemical rearrangement, is described. The proposed reaction mechanism is also discussed.

Synthesis, Bioactivity, and Crystal Structure Analysis of 2-(3-Oxobenzo[d]isothiazol-2(3H)-yl)ethyl Benzoates

Fifteen novel 2-（3-oxobenzo[d]isothiazol-2（3H）-yl）ethyl benzoates were synthesi- zed by the condensation of 2-（2-hydroxyethyl）benzo[d]isothiazol-3（2H）-one with substituted benzoic acids in dichloromethane. All the compounds were characterized by elemental analysis, IR, ESI-MS and 1H NMR. The crystal structures for 2-（2-hydroxyethyl）benzo[d]isothiazol-3（2H）-one （2） and 2-（3-oxobenzo[d]isothiazol-2（3H）-yl）ethyl 2-methoxybenzoate （30） have been determined by X-ray crystal structure analysis. Compound 2 （C9H9NO2S） crystallizes in the monoclinic system, space group Pn with a = 10.552（3）, b = 7.849（2）, c = 10.765（4） A, β = 103.128（4）°, V= 868.3（5） A3, Mr = 195.24, Dc = 1.493 Mg.m-3, μ = 0.33 mm-1, F（000） = 408, Z = 4, R= 0.0314 and wR= 0.0628. Compound 30 （C17H15NO4S） crystallizes in the triclinic system, space group P1 with a = 8.028（2）, b = 9.300（2）, c = 10.430（3）A, V= 752.1（3）A3, Mr = 329.36, D,= 1.454 Mg.m-3, p = 0.24 mm-1, F（000） = 344, Z = 2, R = 0.0377 and wR = 0.0904. The preliminary biological test indicated that the title compounds show better growth inhibitory activity against the gram-positive bacteria than the gram-negative bacteria.

Electrochemical Activation of CO_2 for the Synthesis of Ethyl Carbanilate under Mild Conditions

A novel electrochemical procedure for the synthesis of ethyl carbanilate from aniline and carbon dioxide was developed via the selective cathodic reduction of carbon dioxide in CO2-saturated DMF solution containing 0. 1 mol/L TEABr at room temperature, followed by the addition of Eft as an alkylating agent. The synthesis was carried outun der mild[p（CO2） = 1.0×10^5 Pa, t =20 ℃ ] and safe conditions. Influences of the nature of the electrodes, the current densities, the passed charges during electrolysis, temperatures, and supporting electrolytes on the yield of ethyl carbanilate were studied to optimize the electrolytic conditions. The selectivity of ethyl carbanilate is 100%.

Efficient Synthesis of 2-Ethyl-A-ring Analogues of 19-Nor-1α,25-dihydroxy Vitamin D_3

The novel 19 nor l α ,25 dihydroxy vitamin D 3 analogues possessing an ethyl at the 2 position(4 and 5), were synthesized by coupling 25 hydroxy Windaus Grundmann ketone derivative 20 with A ring synthons(15 and 19) respectively. The enantioselective synthesis of substituted bicyclic hexanes structure A ring synthons, started from all cis 3,5 dihydroxy 4 ethyl 1 (methoxycarbonyl)cyclohexane via lipase catalyzd asymmetrization, was demonstrated.

Synthesis and Crystal Structure of Ethyl 3-(4-Chlorophenyl)-3,4-dihydro-6-methyl-4-oxo-2-(pyrrolidin-1-yl)furo[2,3-d]pyrimidine-5-carboxylate

The crystal structure of the title compound ethyl 3-（4-chlorophenyl）-3,4-dihydro-6- methyl-4-oxo-2-（pyrrolidin-1-yl）furo[2,3-d]pyrimidine-5-carboxylate （C20H20ClN3O4, Mr= 401.84） has been prepared and determined by single-crystal X-ray diffraction. The crystal is of monoclinic, space group P21/n with a = 20.6215（9）, b = 8.5311（4）, c = 21.6886（9） A^°, β = 91.607（1）°, V = 3814.0（3）A^°^3, Z = 8, Dc = 1.400 g/cm^3, F（000） = 1680, μ = 0.233 mm^-1, R = 0.0718 and wR = 0.1545 for 6717 observed reflections with I 〉 2σ（I）. X-ray diffraction analysis reveals two crystallographically independent molecules in the asymmetric unit.

Synthesis, Crystal Structure and Antitumor Activities of N-(2-(1H-indol-3-yl)ethyl)-2-nitroaniline

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.

Optimizing the Synthesis of Ethyl tert-Butyl Ether in Continuous Catalytic Distillation Column Using New Ion Exchange Resin Catalyst

Liquid phase synthesis of one of the important fuel oxygenate, ethyl tert-butyl ether （ETBE）, from etha-nol and tert-butyl alcohol （TBA） has been studied in catalytic distillation column （CDC） using ion exchange resin catalyst CT-145H. A packed CDC of 1.2 m height and 50 mm diameter with indigenously developed reactive sec-tion packing was used to generate experimental data. Effect of different key variables on product purity in distillate, was investigated to find the optimum operating conditions for ETBE synthesis. The optimum conditions for 0.2 kg·s-1 of ethanol feed were found：reboiler duty of 375 W, molar feed ratio of 1︰1.3 of reactants, and reflux ratio of 7. Concentration profiles for each component along each column section at optimum conditions were also drawn. Neither output nor input multiplicity was observed at experimental conditions.

Solvent-free synthesis of some ethyl arylglyoxylates

An efficient and convenient approach to synthesize of ethyl arylglyoxylates by solvent-free grinding was described. Eight ethyl arylglyoxylates had been synthesized by this method, this method provided several advantages such as little pollution, high yield, good selectivity, and simple workup procedure, their structures were confirmed by IR, ^1HNMR.

Synthesis and Crystal Structure of (E)-Ethyl 3-Keto-18β-glycyrrhetinate 3-Oxime

A novel derivative of glycyrrhetinic acid, （E）-ethyl 3-keto-18β-glycyrrhetinate 3- oxime C32H49NO4 （Mr = 511.72）, was synthesized and structurally characterized by IR, 1^H NMR and single-crystal X-ray diffraction. It belongs to monoclinic, space group P21, with a = 12.4897（12）, b = 7.3190（7）, c = 15.9944（14）A, β = 94.833（2）o, V = 1456.9（2）A^3, Z = 2, Dc = 1.167 g/cm^3, μ = 0.075 mm^-1, F（000） = 560, the final R = 0.0449 and wR = 0.1122. A total of 7486 reflections were collected, of which 2785 were independent （Rint = 0.0199） and 2605 were observed with I 〉 2σ（I）. There exists an intermolecular hydrogen bond which helps to stabilize the crystal structure.

Synthesis and Crystal Structure of 1,2-Bis(1-phenyl-3-methylthio- 4-iminopyrazolo[3,4-d]pyrimidin-5-yl) ethane

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 ?.

Synthesis and Anti-influenza Virus Activity of Ethyl 6-Bromo-5-hydroxyindole-3-carboxylate Derivatives

A series of ethyl 6-bromo-5-hydroxyindole-3-carboxylate derivatives were synthesized and their in vitro anti-influenza virus activity was evaluated. All the compounds were characterized by 1H NMR and MS.

Synthesis and Crystal Structure of Ethyl 2-(6-(1,3-Dioxo-4,5,6,7-tetrahydro-1H-isoindol-2(3H)-yl)-7-fluoro-3-oxo-2H-benzo[b][1,4]oxazin-4(3H)-yl) Butanoate

The title compound ethyl 2-（6-（1,3-dioxo-4,5,6,7-tetrahydro-lH-isoindol-2（3H）- yl）-7-fluoro-3-oxo-2H-benzo[b][1,4]oxazin-4（3H）-yl） butanoate 3 was synthesized by the reaction of ethyl 2-（6-amino-7-fluoro-3-oxo-2H-benzo[b][1,4]oxazin-4（3H）-yl） butanoate with 4,5,6,7- tetraydrophthalic anhydride, and its structure was determined by X-ray single-crystal diffraction. The crystal belongs to the monoclinic system, space group P2 1/n with a = 9.3469（2）, b = 16.7715（5）, c = 13.7153（4） A, β= 104.9680（10）°, μ = 0.107 mm^-1, Mr = 430.42, V= 2077.08（10） ,A3, Z= 4, Dc = 1.376 g/cm3, F（000） = 904, T= 296（2） K, R = 0.0508 and wR = 0.1478.

Synthesis of Ethyl 3-Fluoroalkyl-3-Halo Acrylate With CH_2N_2

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.

Synthesis and Crystal Structure of 4-(4,6-Dimethoxylpyrimidin-2-yl)-3-thiourea Carboxylic Acid Ethyl Ester

4-（4,6-Dimethoxyl-pyrimidin-2-yl）-3-thiourea carboxylic acid ethyl ester was synthesized by the reaction of 2-amino-4,6-dimethoxyl pyrimidine, potassium thiocyanate and methyl chloroformate in ethyl acetate. Single crystals suitable for X-ray measurement were obtained by recrystallization with the solvent of dimethyl formamide at room temperature. The crystal structure was determined by X-ray diffraction analysis. Crystallographic data： C10H14N4O4S, M, = 286.31, monoclinic, space group C2/c with a = 2.5309（3）, b = 0.67682（6）, c = 1.74237（19） nm, β = 114.744（3）°, V= 2.7106（5） nm3, Dc = 1.403 g/cm3, p = 0.225 mm-1, F（000） = 1200, Z= 8, R= 0.0514 and wR= 0.1529.