HRID1740102
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 dry ice/acetone bath-chilled solution of 1-(4-bromo-2,6-dimethylphenyl)-3,5-diethyl-1H-pyrazole-4-carboxylic acid methyl ester (1.1 g, 3.1 mmol) in anhydrous tetrahydrofuran (8 ml), diisobutylaluminum hydride (1.0 M in toluene; 10 ml, 10 mmol) was added dropwise. After 15 minutes, the reaction mixture was warmed to 0°-5° C. and stirred at that temperature for 2.5 hours. The reaction was then quenched by addition of 2 ml of water, and the organic solvent was removed in vacuo. Extraction of the residual mixture with ethyl acetate, anhydrous sodium sulfate drying of the resulting extract, and its concentration in vacuo afforded the title compound as a yellow oil (0.77 g).
WORKUP
后处理
- temperaturethe reaction mixture was warmed to 0°-5° C.
- customThe reaction was then quenched by addition of 2 ml of water
- customthe organic solvent was removed in vacuo
- extractionExtraction of the residual mixture with ethyl acetate, anhydrous sodium sulfate
- customdrying of the resulting
- extractionextract
- concentrationits concentration in vacuo