HRID1702059

反应详情

EQUATION

反应方程式

HRID 1702059 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

4

PROCEDURE

实验过程

Trifluoroacetic anhydride (0.1 ml.) and triethylamine (0.2 ml.) were added to a solution of 7-(2-methoxyimino-3,3-ethylenedioxybutyramido)-3-hydroxycepham-4-carboxylic acid (syn isomer, 50 mg.) in dry tetrahydrofuran (5 ml.) and stirred at room temperature for 10 minutes. A sodium bicarbonate aqueous solution (2 ml.) was added to the resultant solution and heated for two minutes. Ethyl acetate and water were added to the solution, acidified with 6 N hydrochloric acid and extracted with ethyl acetate. The aqueous layer was extracted with ethyl acetate. The ethyl acetate layer and extract were combined together, washed with water and a sodium chloride aqueous solution in turn and dried over magnesium sulfate. The solution was evaporated in vacuo, and the residue was pulverized with diethyl ether to give 7-(2-methoxyimino-3,3-ethylenedioxybutyramido)-3-cephem-4-carboxylic acid (syn isomer, 30 mg.)

WORKUP

后处理

  1. temperatureheated for two minutes
  2. extractionextracted with ethyl acetate
  3. extractionThe aqueous layer was extracted with ethyl acetate
  4. extractionThe ethyl acetate layer and extract
  5. washwashed with water
  6. dry with materiala sodium chloride aqueous solution in turn and dried over magnesium sulfate
  7. customThe solution was evaporated in vacuo