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
Lithium aluminium hydride (884 mg) was added to a solution of ethyl 1-(4-benzyloxybenzyl)-3-phenyl-1H-pyrazole-4-carboxylate (9.61 g) in tetrahydrofuran (50 ml) at 0° C., and the mixture was stirred at 0° C. for one hour. After adding water, the reaction mixture was stirred at room temperature for one hour. After the precipitate was removed by filtration, the filtrate was extracted with ethyl acetate. The ethyl acetate layer was washed with saturated aqueous sodium chloride solution, dried (MgSO4), and then concentrated. The crystals obtained were collected by filtration to yield [1-(4-benzyloxybenzyl)-3-phenyl-1H-pyrazol-4-yl]methanol (23.10 g, yield: 97%). This was recrystallized from ethyl acetate-hexane. Melting point: 88–89° C.
WORKUP
后处理
- stirringthe reaction mixture was stirred at room temperature for one hour
- customAfter the precipitate was removed by filtration
- extractionthe filtrate was extracted with ethyl acetate
- washThe ethyl acetate layer was washed with saturated aqueous sodium chloride solution
- dry with materialdried (MgSO4)
- concentrationconcentrated
- customThe crystals obtained
- filtrationwere collected by filtration