HRID869488

反应详情

EQUATION

反应方程式

HRID 869488 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, 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
  4. washwashed twice with a 10% aqueous sodium chloride solution (200 mL)
  5. dry with materialdried over magnesium sulfate
  6. customThe solvent was evaporated