HRID648902

反应详情

EQUATION

反应方程式

HRID 648902 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To 8.2 g of 1-(4-carboethoxyphenyl)-2-mercapto-1,3,4-triazole was added 50 ml of an aqueous solution of 2 mol/liter of sodium hydroxide and the mixture was refluxed for 1 hour. Then, 100 ml of water was added to the reaction mixture and after filtering away insoluble matter, the pH of the filtrate was adjusted to about 1 by the addition of hydrochloric acid. Crystals thus formed were collected by filtration, dissolved in 500 ml of N,N-dimethylformamide and ethyl acetate and hexane were added to the solution, whereby 6.0 g of 1-(4-carboxyphenyl)-2-mercapto-1,3,4-triazole was obtained. The yield was 82.2% and the melting point was above 300° C.

WORKUP

后处理

  1. temperaturethe mixture was refluxed for 1 hour
  2. filtrationafter filtering away insoluble matter
  3. additionthe pH of the filtrate was adjusted to about 1 by the addition of hydrochloric acid
  4. customCrystals thus formed
  5. filtrationwere collected by filtration
  6. dissolutiondissolved in 500 ml of N,N-dimethylformamide
  7. additionethyl acetate and hexane were added to the solution