HRID1986976

反应详情

EQUATION

反应方程式

HRID 1986976 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 stirring at room temperature overnight. 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 a 10% aqueous solution of sodium chloride (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 titled 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 a 10% aqueous solution of sodium chloride (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