HRID1433133

反应详情

EQUATION

反应方程式

HRID 1433133 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

To a suspension of 4-amino-3-chlorophenol (23.7 g) in N,N-dimethylformamide (100 mL) was added pyridine (23.4 mL) while cooling in an ice bath, and phenyl chloroformate (23.2 mL) was added dropwise below 20° C. After stirring at room temperature for 30 min, water (400 mL), ethyl acetate (300 mL), and 6N-HCl (48 mL) were added and stirred. The organic layer was separated off, washed twice with a 10% aqueous sodium chloride solution (200 mL), and dried over magnesium sulfate. The solvent was evaporated to give 46 g of the titled compound as a solid.

WORKUP

后处理

  1. temperaturewhile cooling in an ice bath
  2. stirringstirred
  3. customThe organic layer was separated off
  4. washwashed twice with a 10% aqueous sodium chloride solution (200 mL)
  5. dry with materialdried over magnesium sulfate
  6. customThe solvent was evaporated