HRID742432

反应详情

EQUATION

反应方程式

HRID 742432 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A 4N potassium hydroxide aqueous solution (4.75 liters) was added to an ethanol solution (3 liters) of methyl N-(2-fluoro-4-chloro-5-cyclopentyloxyphenyl)carbamate (2.25 Kg, 7.85 mol), followed by refluxing under heating for 5 hours. After completion of the reaction, the reaction solution was cooled to room temperature, water (5 liters) was added thereto, and the mixture was extracted with toluene (5 liters×2 portions). The organic layer was washed with water and dried over anhydrous magnesium sulfate. The drying agent was separated by filtration, and the filtrate was distilled off under reduced pressure to obtain 2-fluoro-4-chloro-5-cyclopentyloxyaniline as an oily substance (1.75 Kg, 7.62 mol, 98.3% yield). Boiling point: 143°-145° C./1.5 mmHg.

WORKUP

后处理

  1. temperatureby refluxing
  2. temperatureunder heating for 5 hours
  3. customAfter completion of the reaction
  4. extractionthe mixture was extracted with toluene (5 liters×2 portions)
  5. washThe organic layer was washed with water
  6. dry with materialdried over anhydrous magnesium sulfate
  7. customThe drying agent was separated by filtration
  8. distillationthe filtrate was distilled off under reduced pressure