HRID1660587

反应详情

EQUATION

反应方程式

HRID 1660587 反应方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 2,2,2-trichloroethyl 2-methyl-2,3-methylene-6-{2-(2-thienyl)acetamido}penam-3-carboxylate (1.74 g.) in dried dichloromethane (20 ml.) was dropwise added at -15° C. to a solution of aluminum bromide (2.14 g.) in dried dichloromethane (10 ml.) and the mixture was stirred for 4 hours at room temperature. After the reaction, the reaction mixture was washed in turn with 5% hydrochloric acid, water, 5% sodium bicarbonate aqueous solution and water and then dried. After the solvent was distilled off, the residue (powder) was recrystallized from ethanol to give 2,2,2-trichloroethyl 2-methyl-7-{2-(2-thienyl)acetamido}-3-cephem-4-carboxylate (1.46 g.), mp 161° to 162° C. (dec.).

WORKUP

后处理

  1. customAfter the reaction
  2. washthe reaction mixture was washed in turn with 5% hydrochloric acid, water, 5% sodium bicarbonate aqueous solution and water
  3. customdried
  4. distillationAfter the solvent was distilled off
  5. customthe residue (powder) was recrystallized from ethanol