HRID1616094

反应详情

EQUATION

反应方程式

HRID 1616094 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Crude 5-acetamino-4-fluoro-2-methyl-benzenethiol (280 g, 1.41 mol) was added to a 5% (w/w) solution of potassium hydroxide (250 g, 4.46 mol) in water and the mixture was refluxed for 5 hours. The resulting solution was adjusted to pH 7 with dilute hydrochloric acid and was then extracted with ethyl acetate. The organic phase was dried with sodium sulfate and concentrated under reduced pressure to give 5-amino-4-fluoro-2-methyl-benzenethiol as a crude intermediate (160 g, 88%).

WORKUP

后处理

  1. temperaturethe mixture was refluxed for 5 hours
  2. extractionwas then extracted with ethyl acetate
  3. dry with materialThe organic phase was dried with sodium sulfate
  4. concentrationconcentrated under reduced pressure