HRID1065851

反应详情

EQUATION

反应方程式

HRID 1065851 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a stirred solution of 3-[(8-amino-6-tetrazolo[1,5-b]pyridazinyl)thiomethyl]-7-(4-chloro-3-oxobutyramido)-3-cephem-4-carboxylic acid (6.72 g; 0.0171 mole) in acetic acid (60 ml), a solution of sodium nitrite (1.65 g; 0.0239 mole) in water (6 ml) was added at 5°-10° C. After stirring for 3.5 hours at room temperature, the reaction mixture was quenched with brine and extracted with ethyl acetate (4×200 ml). The combined extracts were washed with water, dried over NaSO4 and evaporated to a foam. Trituration of this product with diethyl ether afforded the title compound as a beige powder, 6.3 g.

WORKUP

后处理

  1. customthe reaction mixture was quenched with brine
  2. extractionextracted with ethyl acetate (4×200 ml)
  3. washThe combined extracts were washed with water
  4. dry with materialdried over NaSO4
  5. customevaporated to a foam