HRID1284013

反应详情

EQUATION

反应方程式

HRID 1284013 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

0.7 g of 4-cyclohexyl 2-methylthiocarbamoyl cyclohexanone dissolved in 30 ml ethanol are added with 0.15 g hydrazine hydrate. The mixture is heated to reflux for 30 mn until the evolution of sulphydric gas has ceased. 0.3 ml acetic acid are thereafter added and the whole is refluxed for 3 hours. The mixture is evaporated off giving a yellow liquid as residue. The residue is taken up with ether; the organic solution is washed with a saturated aqueous solution of sodium bicarbonate then with water until the washings are neutral, finally dried and evaporated off. 0.6 g of 5-cyclohexyl 3-methylamino 4,5,6,7-tetrahydroindazole are thus recovered and recrystallized from the minimum amount of isopropanol.

WORKUP

后处理

  1. temperatureThe mixture is heated
  2. temperatureto reflux for 30 mn until the evolution of sulphydric gas
  3. temperaturethe whole is refluxed for 3 hours
  4. customThe mixture is evaporated off
  5. customgiving a yellow liquid as residue
  6. washthe organic solution is washed with a saturated aqueous solution of sodium bicarbonate
  7. customfinally dried
  8. customevaporated off
  9. custom0.6 g of 5-cyclohexyl 3-methylamino 4,5,6,7-tetrahydroindazole are thus recovered
  10. customrecrystallized from the minimum amount of isopropanol