青霉素G亚砜对甲氧基苄酯的合成研究
Study on Synthesis of P-methoxybenzyl Penicillin G Sulfoxide Ester
秦伟 1王静1
作者信息
- 1. 齐齐哈尔医学院,黑龙江齐齐哈尔161000
- 折叠
摘要
目的:合成青霉素G亚砜对甲氧基苄酯(化合物A).方法:以青霉素G钾盐和对甲氧基苄氯(1.1:1)为原料,四丁基溴化铵(TBAB)为催化剂,三氯甲烷/N,N-二甲基甲酰胺(DMF)为溶剂,过氧乙酸为氧化剂合成化合物A,并进行核磁共振结构表征.以收率为指标,确定较佳的酯化反应温度、酯化反应时间、TBAB用量等反应条件.结果:制备得到了化合物A(收率88％,纯度98.5％)并经过结构表征证实.化合物A的最佳反应条件是酯化反应温度为50℃,酯化反应时间为4h,TBAB用量为0.5％.结论:以确定的反应条件可得到目标化合物,合成周期短,利于工业化生产.
Abstract
OBJECTIVE: To synthesize P-methoxybenzyl penicillin G sulfoxide ester (compound A).METHODS: Compound A was synthesized by using potassium penicillin G and P-methoxybenzyl (1.1 ∶ 1) as raw material, tetrabutyl ammonium bromide (TBAB) as catalytic agent, trichloromethane/N, N-dimethylformamide as solvent and peroxyacetic acid as oxidation agent; the structure of it was characterized by NMR.The optimal reaction conditions such as reaction temperature, reaction time, amount of TBAB were well studied with yield as index.RESULTS: Compound A (yield of 88％, purity of 98.5％) were obtained and confirmed.The optimal reaction condition of compound A was as follows: esterification temperature of 50 ℃, esterification time of 4h, TBAB amount of 0.5％.CONCLUSIONS: Target compound could be obtained by this technology.The synthetic cycle is short,which is suitable for industrial production.
关键词
青霉素G钾盐/青霉素G亚砜对甲氧基苄酯/合成Key words
Potassium penicillin G/P-methoxybenzyl penicillin G sulfoxide ester/Synthesis引用本文复制引用
出版年
2013
国家科技期刊平台
NSTL
维普
万方数据