HRID648902
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperaturethe mixture was refluxed for 1 hour
- filtrationafter filtering away insoluble matter
- additionthe pH of the filtrate was adjusted to about 1 by the addition of hydrochloric acid
- customCrystals thus formed
- filtrationwere collected by filtration
- dissolutiondissolved in 500 ml of N,N-dimethylformamide
- additionethyl acetate and hexane were added to the solution