HRID46596

反应详情

EQUATION

反应方程式

HRID 46596 的结构方程式

PROCEDURE

实验过程

A solution of 2.19 g. (10 mmol) of ethyl [(4,5-dihydro-5-thioxo-1H-1,2,4-triazol-3-yl)thio]acetate in 50 ml. of 5% sodium hydroxide was heated at reflux for 1 hour. After thorough cooling, the mixture was filtered, and the filtrate was washed with ethyl acetate. The aqueous layer was separated, acidified to pH 1 and extracted with ethyl acetate. The extract was evaporated in vacuo to dryness. The residue was crystallized from chloroform to give 1.43 g. (75% yield) of [(4,5-dihydro-5-thioxo-1H-1,2,4-triazol-3-yl)thio]acetic acid.

WORKUP

后处理

  1. temperatureat reflux for 1 hour
  2. filtrationAfter thorough cooling, the mixture was filtered
  3. washthe filtrate was washed with ethyl acetate
  4. customThe aqueous layer was separated
  5. extractionextracted with ethyl acetate
  6. customThe extract was evaporated in vacuo to dryness
  7. customThe residue was crystallized from chloroform
  8. customto give 1.43 g