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
CONDITIONS
反应条件
- 温度
- 0 °C
PROCEDURE
实验过程
To a solution (10 mL) of ethyl 5-isobutoxy-1-(2-methylphenyl)-1H-pyrazole-3-carboxylate (1.07 g, 3.54 mmol) in anhydrous tetrahydrofuran was added lithium aluminum hydride (0.13 g, 3.54 mmol) under stirring at 0° C., and the mixture was stirred at the same temperature for 2 hr. After completion of the reaction, sodium sulfate decahydrate (2.28 g, 7.08 mmol) was added to the reaction system and the mixture was stirred at room temperature for 2 hr. The precipitated insoluble material was filtered off, and the filtrate was concentrated under reduced pressure. The residue was purified by silica gel column chromatography (hexane/ethyl acetate=4/1-1/1) to give the title compound (0.85 g, yield 92%) as a pale-yellow oil.
WORKUP
后处理
- stirringthe mixture was stirred at the same temperature for 2 hr
- additionwas added to the reaction system
- stirringthe mixture was stirred at room temperature for 2 hr
- filtrationThe precipitated insoluble material was filtered off
- concentrationthe filtrate was concentrated under reduced pressure
- customThe residue was purified by silica gel column chromatography (hexane/ethyl acetate=4/1-1/1)