An efficient and environmental-friendly one-pot procedure has been developed for the synthesis of 1,3,4-oxadiazole-5- thioethers by the reaction of acylhydrazine with carbon disulfide and organic halides or α, β-uns...An efficient and environmental-friendly one-pot procedure has been developed for the synthesis of 1,3,4-oxadiazole-5- thioethers by the reaction of acylhydrazine with carbon disulfide and organic halides or α, β-unsaturated carbonyl compounds. The reactions were carried out in water in the presence of potassium phosphate within 2-4 h to afford the expected products in excellent yields.展开更多
A new environmental friendly catalyst, H3PW6Mo6O40/TiO2 was prepared. The optimum conditions have been found, that is, mass ratio of m (TiO2): m (H3PW6Mo6O40) is 1:2.0, volume of water is 30 mL, the reflux react...A new environmental friendly catalyst, H3PW6Mo6O40/TiO2 was prepared. The optimum conditions have been found, that is, mass ratio of m (TiO2): m (H3PW6Mo6O40) is 1:2.0, volume of water is 30 mL, the reflux reaction time is 2 h, and activated temperature is 150 ℃. H3PW6Mo6O40/TiO2 was used as catalyst in catalytic synthesis ofacetals and ketals. Effects ofn (aldehyde(ketone)): n (glycol), catalyst dosage and reaction time on yield were investigated. Optimal conditions were: n(aldehyde (ketone)): n (glycol)=1.0 : 1.4; mass fraction of catalyst to reactants, 0.8%; reaction time, 1.0 h and cyclohexane as water-stripped reagent, 10 mL. Under these conditions, yields of acetals and ketals can reach 53.0% -86.9 0%展开更多
Syntheses of 3-substituted coumarins by the condensation reaction of salicylaldehyde with activated methylene compounds (ethyl cyanoacetate, malonic acid) are discussed in media of ionic liquids--(2-hydroxyethyl)a...Syntheses of 3-substituted coumarins by the condensation reaction of salicylaldehyde with activated methylene compounds (ethyl cyanoacetate, malonic acid) are discussed in media of ionic liquids--(2-hydroxyethyl)ammonium carboxylates (formates, acetates, lactates) without utilization of any other catalysts. The dependence of yields of the reaction product is investigated on the structure of ionic liquids (their cations, anions, total polarity and pseudo-pH values). 3-Substituted coumarins are prepared in high yields in media of these environmentally friendly ionic liquids which serve simultaneously as reaction media and as catalysts. The mentioned ionic liquids are prepared by reactions of corresponding hydroxyethyl-amines with carboxylic acids, and their quantitative analyses being made by potentiometric titration of ionic liquids with perchloric acid in 100% acetic acid.展开更多
基金Natural Science Foundation of China (Grant No.20672009)the Major State Basic Research Development Program(Grant No.2004CB719900).
文摘An efficient and environmental-friendly one-pot procedure has been developed for the synthesis of 1,3,4-oxadiazole-5- thioethers by the reaction of acylhydrazine with carbon disulfide and organic halides or α, β-unsaturated carbonyl compounds. The reactions were carried out in water in the presence of potassium phosphate within 2-4 h to afford the expected products in excellent yields.
基金Acknowledgements: This work was financially supported by the Natural Science Foundation of Hubei Province, China (No. 2005ABA053) and the National Natural Science Foundation of China (No. 20471044).
文摘A new environmental friendly catalyst, H3PW6Mo6O40/TiO2 was prepared. The optimum conditions have been found, that is, mass ratio of m (TiO2): m (H3PW6Mo6O40) is 1:2.0, volume of water is 30 mL, the reflux reaction time is 2 h, and activated temperature is 150 ℃. H3PW6Mo6O40/TiO2 was used as catalyst in catalytic synthesis ofacetals and ketals. Effects ofn (aldehyde(ketone)): n (glycol), catalyst dosage and reaction time on yield were investigated. Optimal conditions were: n(aldehyde (ketone)): n (glycol)=1.0 : 1.4; mass fraction of catalyst to reactants, 0.8%; reaction time, 1.0 h and cyclohexane as water-stripped reagent, 10 mL. Under these conditions, yields of acetals and ketals can reach 53.0% -86.9 0%
文摘Syntheses of 3-substituted coumarins by the condensation reaction of salicylaldehyde with activated methylene compounds (ethyl cyanoacetate, malonic acid) are discussed in media of ionic liquids--(2-hydroxyethyl)ammonium carboxylates (formates, acetates, lactates) without utilization of any other catalysts. The dependence of yields of the reaction product is investigated on the structure of ionic liquids (their cations, anions, total polarity and pseudo-pH values). 3-Substituted coumarins are prepared in high yields in media of these environmentally friendly ionic liquids which serve simultaneously as reaction media and as catalysts. The mentioned ionic liquids are prepared by reactions of corresponding hydroxyethyl-amines with carboxylic acids, and their quantitative analyses being made by potentiometric titration of ionic liquids with perchloric acid in 100% acetic acid.