HRID1980422

反应详情

EQUATION

反应方程式

HRID 1980422 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Methanesulphonic acid (37.7 cc) is added in the course of 5 minutes to a solution of 2-benzhydryloxycarbonyl-7-t-butoxycarbonylamino-3-[2-(pyridin-3-yl-amino)thiazol-5-yl]-8-oxo-5-thia-1-azabicyclo[4.2.0]oct-2-ene (37.22 g) in acetonitrile (372 cc). The mixture is stirred for 5 minutes and the reaction solution is then added to a mixture of a saturated solution of sodium bicarbonate (870 cc), distilled water (1,740 cc) and methylene chloride (580 cc). The mixture is stirred for 10 minutes and the precipitate is filtered off and washed with distilled water (4×100 cc). The product is dried to give 7-amino-2-benzhydryloxycarbonyl-3-[2-(pyridin-3-yl-amino)thiazol-5-yl]-8-oxo-5-thia-1-azabicyclo-[4.2.0]oct-2-ene (27.66 g) in the form of a pale yellow crystalline powder.

WORKUP

后处理

  1. distillationdistilled water (1,740 cc) and methylene chloride (580 cc)
  2. stirringThe mixture is stirred for 10 minutes
  3. filtrationthe precipitate is filtered off
  4. washwashed with distilled water (4×100 cc)
  5. customThe product is dried