HRID372864

反应详情

EQUATION

反应方程式

HRID 372864 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a suspension of 27.2 g (0.1 mol) of 7-ACA in 200 ml of water and 100 ml of acetone was added a solution of 18.9 g of sodium bicarbonate in 200 ml of water. The resultant solution was warmed on a steam bath and a solution of 14.5 & (0.125 mol) of 1-methyl-5-mercapto-1,2,3,4-tetrazole in 200 ml of acetone was added. The reaction mixture was refluxed for 3.5 hours while maintaining the pH at 7.4-8.0 by addition of 5% sodium bicarbonate solution. Acidification of the cooled reaction mixture to pH 3.5 with 6N hydrochloric acid resulted in precipitation of 7 -amino-3-(1-methyl-1,2,3,4-tetrazole-5-ylthiomethyl)-3-cephem-4-carboxylic acid which was collected, washed (H2 0), and air dried (16 g, 49%).

WORKUP

后处理

  1. temperatureThe reaction mixture was refluxed for 3.5 hours
  2. temperaturewhile maintaining the pH at 7.4-8.0