HRID557485

反应详情

EQUATION

反应方程式

HRID 557485 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

After dissolving phenyl N-(2-chloro-4-hydroxyphenyl)carbamate in N,N-dimethylformamide (100 mL), cyclopropylamine (22.7 mL) was added while cooling on ice and the mixture was stirred overnight at room temperature. Water (400 mL), ethyl acetate (300 mL) and 6N HCl (55 mL) were then added, the mixture was stirred and the organic layer was separated. The organic layer was washed twice with 10% brine (200 mL), and dried over magnesium sulfate. Prism crystals obtained by concentrating the solvent were filtered and washed with heptane to give 22.8 g of the title compound (77% yield from 4-amino-3-chlorophenol).

WORKUP

后处理

  1. additionwas added
  2. temperaturewhile cooling on ice
  3. stirringthe mixture was stirred
  4. customthe organic layer was separated
  5. washThe organic layer was washed twice with 10% brine (200 mL)
  6. dry with materialdried over magnesium sulfate
  7. customPrism crystals obtained
  8. concentrationby concentrating the solvent
  9. filtrationwere filtered
  10. washwashed with heptane