A novel synthesis process of 5H-dibenz[b,f]azepine was studied.It is an important intermediate of 5H-dibenz[b,f]azepine-5-carboxamide,used in genetic engineering,materials science and so on.With 10,11-dihydro-5H-diben...A novel synthesis process of 5H-dibenz[b,f]azepine was studied.It is an important intermediate of 5H-dibenz[b,f]azepine-5-carboxamide,used in genetic engineering,materials science and so on.With 10,11-dihydro-5H-dibenz[b,f]azepine as raw material,5-chloroformyl-5H-dibenz[b,f]azepine was prepared by reflux with triphosgene in toluene,brominated with bromine in chlorobenzene,and dehydrobrominated at 130℃,finally,the title compound was obtained by removing chloroformyl group with NaOH in isopropanol with 80.4% overall yield.The optimal reaction conditions and yields (temperature,time,molar yield) were as follows: acyl chlorination,110℃,10 h,93.0%; bromination,dehydrobromination,100℃,2 h,130℃,5 h,88.0%; removal of chloroformyl group,40℃,3 h,98.2%. The melting point of the title compound was the same as literature reported,and its structure was confirmed by 1H NMR.The optimal technology condition to remove chloroformyl group as protection group and its application of protection for some amine compounds were also studied.展开更多
以壳聚糖和2,3-环氧丙基三甲基氯化铵为原料,制备得到壳聚糖季铵盐(HTCC),继而HTCC与乙酰氯、氯乙酰氯和苯甲酰氯反应得到一系列酰基化壳聚糖季铵盐(AHTCC,CAHTCC,BAHTCC).用FT-IR和13 C NMR光谱对产物结构进行了表征,并测试了其抑菌活...以壳聚糖和2,3-环氧丙基三甲基氯化铵为原料,制备得到壳聚糖季铵盐(HTCC),继而HTCC与乙酰氯、氯乙酰氯和苯甲酰氯反应得到一系列酰基化壳聚糖季铵盐(AHTCC,CAHTCC,BAHTCC).用FT-IR和13 C NMR光谱对产物结构进行了表征,并测试了其抑菌活性,结果表明,酰基化修饰的壳聚糖季铵盐抑菌活性较HTCC和壳聚糖原料均有明显提高.原因应该与酰基化HTCC衍生物结构有关,其结构中具有季铵盐结构和酰基结构,亲水基团与疏水基团的同时存在对抑菌活性的提高起到了关键作用.展开更多
Water-soluble diol-functionalized imidazolium ionic liquid 1, prepared from 2,2-bis（1-methyl-methyl-imida- zolium）propane-l,3-diol bromide, potassium hydroxide, and malononitrile, was used as an efficient phosphine-...Water-soluble diol-functionalized imidazolium ionic liquid 1, prepared from 2,2-bis（1-methyl-methyl-imida- zolium）propane-l,3-diol bromide, potassium hydroxide, and malononitrile, was used as an efficient phosphine-free ligand for palladium-catalyzed arylation of aryl halides with acrylates in aqueous phase under mild conditions. It was found that the synergistic coordinating action of diol-functionalized imidazolium cation with CN-containing anion played the key role in improving the activity and stability of the catalyst.展开更多
文摘A novel synthesis process of 5H-dibenz[b,f]azepine was studied.It is an important intermediate of 5H-dibenz[b,f]azepine-5-carboxamide,used in genetic engineering,materials science and so on.With 10,11-dihydro-5H-dibenz[b,f]azepine as raw material,5-chloroformyl-5H-dibenz[b,f]azepine was prepared by reflux with triphosgene in toluene,brominated with bromine in chlorobenzene,and dehydrobrominated at 130℃,finally,the title compound was obtained by removing chloroformyl group with NaOH in isopropanol with 80.4% overall yield.The optimal reaction conditions and yields (temperature,time,molar yield) were as follows: acyl chlorination,110℃,10 h,93.0%; bromination,dehydrobromination,100℃,2 h,130℃,5 h,88.0%; removal of chloroformyl group,40℃,3 h,98.2%. The melting point of the title compound was the same as literature reported,and its structure was confirmed by 1H NMR.The optimal technology condition to remove chloroformyl group as protection group and its application of protection for some amine compounds were also studied.
文摘以壳聚糖和2,3-环氧丙基三甲基氯化铵为原料,制备得到壳聚糖季铵盐(HTCC),继而HTCC与乙酰氯、氯乙酰氯和苯甲酰氯反应得到一系列酰基化壳聚糖季铵盐(AHTCC,CAHTCC,BAHTCC).用FT-IR和13 C NMR光谱对产物结构进行了表征,并测试了其抑菌活性,结果表明,酰基化修饰的壳聚糖季铵盐抑菌活性较HTCC和壳聚糖原料均有明显提高.原因应该与酰基化HTCC衍生物结构有关,其结构中具有季铵盐结构和酰基结构,亲水基团与疏水基团的同时存在对抑菌活性的提高起到了关键作用.
基金the National Natural Science Foundation of China （No. 20676033）, the China Post- doctoral Science Foundation （No. 20070410169） and the Shanghai Leading Academic Discipline Project （No. B507） for financial support.
文摘Water-soluble diol-functionalized imidazolium ionic liquid 1, prepared from 2,2-bis（1-methyl-methyl-imida- zolium）propane-l,3-diol bromide, potassium hydroxide, and malononitrile, was used as an efficient phosphine-free ligand for palladium-catalyzed arylation of aryl halides with acrylates in aqueous phase under mild conditions. It was found that the synergistic coordinating action of diol-functionalized imidazolium cation with CN-containing anion played the key role in improving the activity and stability of the catalyst.
