(Z或E)-4-氯-2-对硝基苄氧羰基甲氧亚胺-3-氧代丁酸的合成研究

以2-对硝基苄氧羰基甲氧亚胺基-3-氧代丁酸、磺酰氯为起始原料,在一定条件下经过反应、处理,得到(顺式或反式)即(Z或E)-4-氯-2-对硝基苄氧羰基甲氧亚胺-3-氧代丁酸。通过红外、核磁共振对其结构进行了表征。较佳工艺条件:原料摩尔比n(2-对硝基苄氧羰基甲氧亚胺基-3-氧代丁酸)∶n(磺酰氯)=1∶1.4,在50~55℃反应5~6 h,反应完调节体系pH值为6.5±0.1,顺式、反式异构体产品分离效果达到99%以上,收率分别是24%和48%,纯度均为98%。

Study on synthesis of (Z or E)-4-chloro-2-p-nitrobenzyloxy-carbonyl-methoxyimino-3-oxo-butyric acid

Using 2-p-nitrobenzy-loxycarbonylmethoxyimino-3-oxo-butyric acid,sulfuryl chloride as base material,under the certain conditions,(Z or E)-4-chloro-2-p-nitrobenzyloxy-carbonyl-methoxyimino-3-oxo-butyric acid was synthesized.Its chemical structure was characterized by IR and 1H NMR.The better technology has been obtaind as follows ∶ the mole ratio of n(2-p-nitrobenzy-loxycarbonylmethoxyimino-3-oxo-butyric acid) ∶ n(sulfuryl chloride )=1 ∶ 1.4,reaction time is 5~ 6 h at 50~55 ℃.After finish reaction system dispose of the technology pH is 6.5±0.1,the separating effect reach over 99%,the yield of the product is 24% and 48%,the purity is all 98%.