HRID2253991

反应详情

EQUATION

反应方程式

HRID 2253991 反应方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Sodium 5-mercapto-1,2,3-thiadiazole (2.45 g) was suspended in methanol (20 ml), and a solution of p-methoxybenzyl 7-amino-3-chloromethyl-3-cephem-4-carboxylate (5.60 g) in methylene chloride (20 ml) was added dropwise. The mixture was stirred for 30 min. under ice-cooling, an insoluble material was filtered off, and the solvent was evaporated to obtain a crude material (6.38 g). The crude material was subjected to silica gel chromatography eluting with chloroform-ethyl acetate to obtain p-methoxybenzyl 7-amino-3-(1,2,3-thiadiazol-5-yl)thiomethyl-3-cephem-4-carboxylate (4.90 g).

WORKUP

后处理

  1. temperaturecooling
  2. filtrationan insoluble material was filtered off
  3. customthe solvent was evaporated
  4. customto obtain a crude material (6.38 g)
  5. washeluting with chloroform-ethyl acetate