HRID583146

反应详情

EQUATION

反应方程式

HRID 583146 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

The methyl 4-amino-3-chloro-5-methoxyiminomethylbenzoate made in the previous step was dissolved in a mixture of 25 ml of methanol and 8 g ml of 10% of aqueous sodium hydroxide and the solution was then was refluxed for 2 hours. The methanol was removed using a rotary evaporator and the residue was partitioned between 25 ml of water and 25 ml of methylene chloride. To the cooled aqueous layer was added 6N aqueous hydrochloric acid, dropwise, with stirring, until the pH of mixture reached a value of 1. The resulting solid was filtered and dried yielding 1.4 g 4-amino-3-chloro-5-methoxyiminomethylbenzoic acid used without further purification.

WORKUP

后处理

  1. temperaturethe solution was then was refluxed for 2 hours
  2. customThe methanol was removed
  3. customa rotary evaporator
  4. customthe residue was partitioned between 25 ml of water and 25 ml of methylene chloride
  5. additionTo the cooled aqueous layer was added 6N aqueous hydrochloric acid
  6. filtrationThe resulting solid was filtered
  7. customdried