HRID1275463

反应详情

EQUATION

反应方程式

HRID 1275463 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
60 °C

PROCEDURE

实验过程

0.75 Gram (2.3 mmol) of 4-ethylthio-5-methyl-6-ethoxycarbonyl-8-chlorothiochroman, 0.47 g (7.1 mmol) of potassium hydroxide, 5 ml of ethanol and 2 ml of water were mixed, and the mixture was stirred under heat at 60° C. for 2 hours. After the completion of the reaction, the solvent was distilled off, 5 ml of water was added, and then 2N hydrochloric acid was added to adjust a pH of 1. Then, the mixture was extracted with ethyl acetate twice. An organic layer was washed with a saturated sodium chloride aqueous solution and dried over anhydrous sodium sulfate, and the solvent was distilled off to give 1.0 g (yield 100%) of 4-ethylthio-5-methyl-6-carboxy-8-chlorothiochroman.

WORKUP

后处理

  1. customAfter the completion of the reaction
  2. distillationthe solvent was distilled off
  3. addition5 ml of water was added
  4. addition2N hydrochloric acid was added
  5. extractionThen, the mixture was extracted with ethyl acetate twice
  6. washAn organic layer was washed with a saturated sodium chloride aqueous solution
  7. dry with materialdried over anhydrous sodium sulfate
  8. distillationthe solvent was distilled off