HRID244657
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 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
- temperaturethe mixture heated
- temperatureat reflux under nitrogen for 58 h
- temperatureheated
- temperatureat reflux under Nitrogen for 72 h
- customthe solvent was removed in vacuo
- additionToluene (15 ml) was added
- customthe solvent removed in vacuo
- customto give a white solid
- customthat was dried in a vacuum oven overnight