HRID973046

反应详情

EQUATION

反应方程式

HRID 973046 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

11.9 g. Prop-2-ynyl bromide was added to a solution of 14.3 g. 5-mercapto-3-isopropyl-1,2,4-triazole in sodium methoxide solution (2.3 g. sodium dissolved in 200 ml. methanol). Then the solution was boiled under reflux for 2 1/2 hours. The solvent was evaporated under reduced pressure from the steam bath and the residual solid triturated with 500 ml. cold water, filtered off and dried under vacuum to give 3-isopropyl-5-prop-2-ynylthio-1,2,4-triazole which was purified by recrystallisation in the presence of charcoal, from petroleum ether (boiling point 80°-100° C.). The melting point of the product was 91°-92° C.

WORKUP

后处理

  1. temperatureunder reflux for 2 1/2 hours
  2. customThe solvent was evaporated under reduced pressure from the steam bath
  3. customthe residual solid triturated with 500 ml
  4. filtrationcold water, filtered off
  5. customdried under vacuum