HRID5156

反应详情

EQUATION

反应方程式

HRID 5156 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
20 °C

PROCEDURE

实验过程

A mixture of 2.6 g of 3-methylthiomethyl-7-amino-ceph -3-eme-4-carboxylic acid, 26 ml of methylene chloride and 3 ml of triethylamine was stirred at 20° C. under an inert atmosphere and after cooling the mixture to -20° C., an acetone suspension of the mixed anhydride of Example 3 prepared from 6 g of the triethylamine salt of the syn isomer of 2-(2-tritylamino-4-thiazolyl)-2-methoxyimino-acetic acid was added thereto. The mixture was stirred for 2 hours at 0° C. and was then acidified with 1 ml of acetic acid. The mixture was evaporated to dryness under reduced pressure and the residue was taken up in 50 ml of methylene chloride. The organic solution was washed with water, dried and evaporated to dryness under reduced pressure. The residue was taken up in 50 ml of ether and the mixture was vacuum filtered to obtain 8.06 g of syn isomer of 3-methylthiomethyl-7-[2-(2 -tritylamino-4-thiazolyl)-2-methoxyimino-acetamido]-ceph-3-eme-4-carboxylic acid.

WORKUP

后处理

  1. temperatureafter cooling the mixture to -20° C.
  2. additionwas added
  3. stirringThe mixture was stirred for 2 hours at 0° C.
  4. customThe mixture was evaporated to dryness under reduced pressure
  5. washThe organic solution was washed with water
  6. customdried
  7. customevaporated to dryness under reduced pressure
  8. filtrationfiltered