HRID434935

反应详情

EQUATION

反应方程式

HRID 434935 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

7-{2-(2-Formamido-4-thiazolyl)-2-methoxyiminoacetamido}-3-chloro-3-cephem-4-carboxylic acid (syn isomer, 0.4 g.) was suspended in methanol (15 ml.). After adding conc-hydrochloric acid (0.16 g.) to the suspension, the mixture was stirred at room temperature for 2.5 hours. Methanol was distilled off from the resultant mixture under reduced pressure, and the residue was dissolved in water (15 ml.). The solution was washed with ethyl acetate (30 ml.) and dichloromethane (30 ml.) in turn. To the acqueous layer was introduced nitrogen gas to remove the remaining organic solvent completely, and the solution was lyophilized to give 7-{2-(2-amino-4-thiazolyl)-2-methoxyiminoacetamido}-3-chloro-3-cephem-4-carboxylic acid hydrochloride (syn isomer 0.35 g.), m.p. 170° to 180° C. (dec.)

WORKUP

后处理

  1. distillationMethanol was distilled off from the resultant mixture under reduced pressure
  2. dissolutionthe residue was dissolved in water (15 ml.)
  3. washThe solution was washed with ethyl acetate (30 ml.) and dichloromethane (30 ml.) in turn
  4. additionTo the acqueous layer was introduced nitrogen gas
  5. customto remove the remaining organic solvent completely