HRID1389684

反应详情

EQUATION

反应方程式

HRID 1389684 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
60 °C

PROCEDURE

实验过程

In water (30 ml) were dissolved 7β-amino-3-(3-oxobutyryloxy)methyl-3-cephem-4-carboxylic acid (3.14 g), sodium hydrogen carbonate (1.84 g) and 5-mercapto-1-methyl-1H-tetrazole (1.4 g) and the solution was adjusted its pH to 5.5, followed by stirring and heating at 60° C. for one hour. After cooling, the reaction solution was washed with dichloromethane (20 ml) and the aqueous layer was adjusted to pH 3.3, followed by stirring for one hour under ice-cooling. The resultant precipitates were collected by filtration and washed with water, methanol and acetone in this order, followed by drying to give 7β-amino-3-(1-methyl-1H-tetrazol-5-yl)thiomethyl-3-cephem-4-carboxylic acid (2.7 g).

WORKUP

后处理

  1. temperatureAfter cooling
  2. washthe reaction solution was washed with dichloromethane (20 ml)
  3. stirringby stirring for one hour under ice-
  4. temperaturecooling
  5. customThe resultant precipitates
  6. filtrationwere collected by filtration
  7. washwashed with water, methanol and acetone in this order
  8. customby drying