HRID869489

反应详情

EQUATION

反应方程式

HRID 869489 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of phenyl N-(2-chloro-4-hydroxyphenyl)carbamate in N,N-dimethylformamide (100 mL) was added cyclopropylamine (22.7 mL) while cooling in an ice bath, and the stirring was continued at room temperature overnight. Water (400 mL), ethyl acetate (300 mL), and 6N—HCl (55 mL) were added thereto, and the mixture was stirred. The organic layer was then separated, washed twice with a 10% aqueous sodium chloride solution (200 mL), and dried over magnesium sulfate. The solvent was evaporated to give prism crystals, which were collected by filtration and washed with heptane to give 22.8 g of the titled compound (yield from 4-amino-3-chlorophenol: 77%).

WORKUP

后处理

  1. temperaturewhile cooling in an ice bath
  2. customThe organic layer was then separated
  3. washwashed twice with a 10% aqueous sodium chloride solution (200 mL)
  4. dry with materialdried over magnesium sulfate
  5. customThe solvent was evaporated
  6. customto give prism crystals, which
  7. filtrationwere collected by filtration
  8. washwashed with heptane