HRID244616

反应详情

EQUATION

反应方程式

HRID 244616 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Methyl 1,4-dimethyl-1H-pyrazole-5-carboxylate (171 mg) was dissolved in 1,4-dioxane (2 ml). Hydrochloric acid (2 ml) was added and the mixture was heated at reflux for 70 h. One drop of concentrated hydrochloric acid was added and the mixture heated at reflux for 45 h. The solution was left to cool and then the solvent was removed in vacuo. To the residue toluene (15 ml) was added and the solvent was removed in vacuo. The solid was dried in a vacuum oven overnight to give the title compound (132 mg) as a white solid.

WORKUP

后处理

  1. temperaturethe mixture was heated
  2. temperatureat reflux for 70 h
  3. temperaturethe mixture heated
  4. temperatureat reflux for 45 h
  5. waitThe solution was left
  6. temperatureto cool
  7. customthe solvent was removed in vacuo
  8. additionTo the residue toluene (15 ml) was added
  9. customthe solvent was removed in vacuo
  10. customThe solid was dried in a vacuum oven overnight