采用1,4-二羰基化合物和伯胺经Paal-Knorr反应制备吡咯衍生物,在100℃的甲苯溶剂中加热回流,运用分水器分出反应中生成的水,以高收率合成了13种2,5-二甲基吡咯衍生物.所有未知化合物经1 H NMR、13 C NMR和质谱进行了表征,同时通过单晶X...采用1,4-二羰基化合物和伯胺经Paal-Knorr反应制备吡咯衍生物,在100℃的甲苯溶剂中加热回流,运用分水器分出反应中生成的水,以高收率合成了13种2,5-二甲基吡咯衍生物.所有未知化合物经1 H NMR、13 C NMR和质谱进行了表征,同时通过单晶X-射线衍射法测定了化合物k和m的晶体结构.展开更多
An efficient and facile method for the synthesis of N-substituted pyrroles in moderate to good yields by the Paal-Knorr reaction of β-diketones with amines in the presence of β-cyclodextrin in aqueous media has been...An efficient and facile method for the synthesis of N-substituted pyrroles in moderate to good yields by the Paal-Knorr reaction of β-diketones with amines in the presence of β-cyclodextrin in aqueous media has been developed. Moreover, this process tolerated diamines （e.g., para-, metaor orthophenylenediamine） to construct bis-pyrrole or mono-pyrrole derivates.β-Cyclodextrin can be recovered easily after the reactions and reused without evident loss in activity.展开更多
2,3,4,6-Tetra-O-acetyl-α-D-galactopyranosyl bromide reacted with carboxylic acids in the presence of CaH_2 and Ag_2CO_3 and small amount of I_2 to give good yields of l-O-acyl-β-D- galactopyranose tetraaeetates.β-A...2,3,4,6-Tetra-O-acetyl-α-D-galactopyranosyl bromide reacted with carboxylic acids in the presence of CaH_2 and Ag_2CO_3 and small amount of I_2 to give good yields of l-O-acyl-β-D- galactopyranose tetraaeetates.β-Anomers of glycosyl esters were obtained by this improved Koenigs-Knorr method.展开更多
A one-pot approach to ethyl 1,4,5-triaryl-lH-pyrazole-3-carboxylates has been developed in moderate to high yields. The tert-BuOLi-mediated Claisen condensation of 1,2-diarylethanones and ethyl oxalyl chloride efficie...A one-pot approach to ethyl 1,4,5-triaryl-lH-pyrazole-3-carboxylates has been developed in moderate to high yields. The tert-BuOLi-mediated Claisen condensation of 1,2-diarylethanones and ethyl oxalyl chloride efficiently provided the enolized lithium salts of ethyl 2,4-dioxo-3,4-diarylbutanoates, which in situ reacted with arylhydrazine hydrochlorides via a hydrochloric acid-promoted Knorr reaction to produce the exquisite triarylpyrazole-3- carboxylates. The procedure promises a convenient access to this highly crowded framework for drug discovery.展开更多
The treatment ofα-bromoalkyl aryl ketones and 2-(propan-2-ylidene)hydrazine carbothioamide afforded 4-aryl-2-(2-(propan-2-ylidene)hydrazinyl)thiazoles via a Hantzsch-thiazole synthesis,which reacted with 4-aryl-2,4-d...The treatment ofα-bromoalkyl aryl ketones and 2-(propan-2-ylidene)hydrazine carbothioamide afforded 4-aryl-2-(2-(propan-2-ylidene)hydrazinyl)thiazoles via a Hantzsch-thiazole synthesis,which reacted with 4-aryl-2,4-diketoesters via a sequential Knorr-pyrazole reaction to deliver a variety of aryl-substituted ethyl 1-(thiazol-2-yl)-1Hpyrazole-3-carboxylates in a one-pot fashion with moderate to high yields.The key intermediates 4-aryl-2,4-diketoesters,existing as its enolic lithium salt,were synthesized in situ by a high-yield tert-BuOLi-mediated Claisen condensation of alkylphenones and diethyl oxalate.This class of elegant molecule comprises aryl groups on the two different heterocyclic cores,and the configurations of two representative molecules were determined by single crystal X-ray crystallography.展开更多
文摘采用1,4-二羰基化合物和伯胺经Paal-Knorr反应制备吡咯衍生物,在100℃的甲苯溶剂中加热回流,运用分水器分出反应中生成的水,以高收率合成了13种2,5-二甲基吡咯衍生物.所有未知化合物经1 H NMR、13 C NMR和质谱进行了表征,同时通过单晶X-射线衍射法测定了化合物k和m的晶体结构.
基金the National Natural Science Foundation of China(No.21172175)Natural Science Foundation of Zhejiang Province(Nos.LY12B02011 and Y4110491)for financial support
文摘An efficient and facile method for the synthesis of N-substituted pyrroles in moderate to good yields by the Paal-Knorr reaction of β-diketones with amines in the presence of β-cyclodextrin in aqueous media has been developed. Moreover, this process tolerated diamines （e.g., para-, metaor orthophenylenediamine） to construct bis-pyrrole or mono-pyrrole derivates.β-Cyclodextrin can be recovered easily after the reactions and reused without evident loss in activity.
文摘2,3,4,6-Tetra-O-acetyl-α-D-galactopyranosyl bromide reacted with carboxylic acids in the presence of CaH_2 and Ag_2CO_3 and small amount of I_2 to give good yields of l-O-acyl-β-D- galactopyranose tetraaeetates.β-Anomers of glycosyl esters were obtained by this improved Koenigs-Knorr method.
基金The authors are grateful to the National Natural Science Foundation of China (Nos.21176074 and 21171093) for financial support
文摘A one-pot approach to ethyl 1,4,5-triaryl-lH-pyrazole-3-carboxylates has been developed in moderate to high yields. The tert-BuOLi-mediated Claisen condensation of 1,2-diarylethanones and ethyl oxalyl chloride efficiently provided the enolized lithium salts of ethyl 2,4-dioxo-3,4-diarylbutanoates, which in situ reacted with arylhydrazine hydrochlorides via a hydrochloric acid-promoted Knorr reaction to produce the exquisite triarylpyrazole-3- carboxylates. The procedure promises a convenient access to this highly crowded framework for drug discovery.
基金The authors are grateful to the National Natural Science Foundation of China(Nos.21176074 and 21171093)for financial support.
文摘The treatment ofα-bromoalkyl aryl ketones and 2-(propan-2-ylidene)hydrazine carbothioamide afforded 4-aryl-2-(2-(propan-2-ylidene)hydrazinyl)thiazoles via a Hantzsch-thiazole synthesis,which reacted with 4-aryl-2,4-diketoesters via a sequential Knorr-pyrazole reaction to deliver a variety of aryl-substituted ethyl 1-(thiazol-2-yl)-1Hpyrazole-3-carboxylates in a one-pot fashion with moderate to high yields.The key intermediates 4-aryl-2,4-diketoesters,existing as its enolic lithium salt,were synthesized in situ by a high-yield tert-BuOLi-mediated Claisen condensation of alkylphenones and diethyl oxalate.This class of elegant molecule comprises aryl groups on the two different heterocyclic cores,and the configurations of two representative molecules were determined by single crystal X-ray crystallography.
