HRID1287330

反应详情

EQUATION

反应方程式

HRID 1287330 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

5

PROCEDURE

实验过程

To a solution of 2,2,2-trichloroethyl 2-methyl-2,3-methylene-6-[2-phenyl-2-(2-chlorophenoxy)acetamido]penam-3-carboxylate (1.18 g.) in a mixture of dimethylformamide (5 ml.) and acetic acid (1.5 ml.) was added zinc powder (1.2 g.) under ice-cooling, and the mixture was stirred for 1.5 hours. After the reaction, the residue (0.65 g.) obtained by post-treating the reaction mixture in the similar manner as described in Example 1 was dissolved in methanol (2 ml.) and a solution of N,N'-dibenzylethylenediamine diacetate (0.20 g.) in water (10 ml.) was added to the solution. Crystals obtained in this manner were dissolved in methanol and subjected to reprecipitation with water to give N,N'-dibenzylethylenediamine salt of 2-methyl-2,3-methylene-6-[2-phenyl-2-(2-chlorophenoxy)acetamido]penam-3-carboxylic acid (0.55 g.), mp 107° to 110°C (dec.)

WORKUP

后处理

  1. temperaturecooling
  2. customAfter the reaction
  3. customthe residue (0.65 g.) obtained
  4. additionby post-treating the reaction mixture in the similar manner
  5. customCrystals obtained in this manner
  6. customsubjected to reprecipitation with water