HRID1680019

反应详情

EQUATION

反应方程式

HRID 1680019 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of 2.5 g (0.00354 mole) of benzyl 6-amino-1'-methyl-spiro[penam-2,4'-piperidine]-3-carboxylate di-p-toluenesulfonate (obtained in 8.1) in 1.5 liter of ethanol is subjected to hydrogenolysis in a Parr's apparatus under 3.2 kg/cm2 of hydrogen in the presence of 2 g of palladium on carbon (10% Pd). After 90 minutes, the reaction mixture is filtered and the filtrate is evaporated to dryness and lyophilized in 600 ml of water. 1.8 g of 6-amino-1'-methyl-spiro[penam-2,4'-piperidine]-3-carboxylic acid di-p-toluenesulfonate is obtained; yield: 83%; M.P. approx 155°-160° C. (start of decomposition).

WORKUP

后处理

  1. filtrationthe reaction mixture is filtered
  2. customthe filtrate is evaporated to dryness