HRID244657

反应详情

EQUATION

反应方程式

HRID 244657 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of ethyl 4-fluoro-1-(1-methylethyl)-1H-pyrazole-5-carboxylate (100 mg) in 1,4-dioxane (2 ml) was added 2M hydrochloric acid (2 ml) and the mixture heated at reflux under nitrogen for 58 h, allowed to stand at room temperature for 62 h, then heated at reflux under Nitrogen for 72 h. The mixture was cooled to room temperature and the solvent was removed in vacuo. Toluene (15 ml) was added and the solvent removed in vacuo to give a white solid that was dried in a vacuum oven overnight to give the title compound (20 mg) as a white solid.

WORKUP

后处理

  1. temperaturethe mixture heated
  2. temperatureat reflux under nitrogen for 58 h
  3. temperatureheated
  4. temperatureat reflux under Nitrogen for 72 h
  5. customthe solvent was removed in vacuo
  6. additionToluene (15 ml) was added
  7. customthe solvent removed in vacuo
  8. customto give a white solid
  9. customthat was dried in a vacuum oven overnight