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
采用高效液相色谱法在装有大环糖肽抗生素键合相的手性柱上拆分了7种氨基带有芴甲氧羰基(fluo reny l-m ethoxycarbony l,Fm o c)保护的氨基酸对映体。比较了Fm o c-缬氨酸和相应的不带保护基的缬氨酸对映体在不同流动相体系中的色谱保...采用高效液相色谱法在装有大环糖肽抗生素键合相的手性柱上拆分了7种氨基带有芴甲氧羰基(fluo reny l-m ethoxycarbony l,Fm o c)保护的氨基酸对映体。比较了Fm o c-缬氨酸和相应的不带保护基的缬氨酸对映体在不同流动相体系中的色谱保留行为;考察了甲醇-醋酸-三乙胺流动相体系中醋酸和三乙胺的浓度以及它们二者的浓度之比对N-Fm o c氨基酸对映体拆分效果的影响。实验结果表明分离温度及流动相流速的变化也会对分离结果产生影响。该法简便快速,已成功地用于这类氨基酸的光学纯度测定。展开更多
The 2% cross linked poly[styrene(iodoso diacetate)] was synthesized, which was used as oxidative reagent from semicarbazones of ketones to the corresponding ketones in wet acetonitrile under mild conditions, and the p...The 2% cross linked poly[styrene(iodoso diacetate)] was synthesized, which was used as oxidative reagent from semicarbazones of ketones to the corresponding ketones in wet acetonitrile under mild conditions, and the possible mechanism was discussed.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.
文摘采用高效液相色谱法在装有大环糖肽抗生素键合相的手性柱上拆分了7种氨基带有芴甲氧羰基(fluo reny l-m ethoxycarbony l,Fm o c)保护的氨基酸对映体。比较了Fm o c-缬氨酸和相应的不带保护基的缬氨酸对映体在不同流动相体系中的色谱保留行为;考察了甲醇-醋酸-三乙胺流动相体系中醋酸和三乙胺的浓度以及它们二者的浓度之比对N-Fm o c氨基酸对映体拆分效果的影响。实验结果表明分离温度及流动相流速的变化也会对分离结果产生影响。该法简便快速,已成功地用于这类氨基酸的光学纯度测定。
文摘The 2% cross linked poly[styrene(iodoso diacetate)] was synthesized, which was used as oxidative reagent from semicarbazones of ketones to the corresponding ketones in wet acetonitrile under mild conditions, and the possible mechanism was discussed.
