CAJ | 학술논문

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%.
이2-대초기변양탄기갑양아알기-3-양대정산、광선록위기시원료,재일정조건하경과반응、처리,득도(순식혹반식)즉(Z혹E)-4-록-2-대초기변양탄기갑양아알-3-양대정산.통과홍외、핵자공진대기결구진행료표정.교가공예조건:원료마이비n(2-대초기변양탄기갑양아알기-3-양대정산):n(광선록)=1:1.4,재50~55 ℃반응5~6 h,반응완조절체계pH치위6.5±0.1,순식、반식이구체산품분리효과체도99%이상,수솔분별시24%화48%,순도균위98%.
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%.