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
A solution of methyl 2-methyl-1-{[2-methyl-3-(trifluoromethyl)phenyl]methyl}-6-(4-morpholinyl)-1H-benzimidazole-4-carboxylate, prepared as described in Example 30 (0.37 g, 0.827 mmol) in Tetrahydrofuran (THF) (10 mL) was cooled to 0° C. LiAlH4 (0.038 g, 1 mmol) in THF (3 mL) was added in and the reaction mixture was stirred at 0° C. for 30 min. The reaction mixture was quenched with water (0.04 mL), NaOH (15%, 0.04 mL) then water (0.12 mL). Anhydrous MgSO4 was added and the reaction mixture was filtered through celite and washed with EtOAc. Evaporation of the solvent gave the crude product. The crude product was purified on a silica column (1-4% MeOH/DCM) to give the solid (0.32 g, 88%).
WORKUP
后处理
- customThe reaction mixture was quenched with water (0.04 mL), NaOH (15%, 0.04 mL)
- additionAnhydrous MgSO4 was added
- filtrationthe reaction mixture was filtered through celite
- washwashed with EtOAc
- customEvaporation of the solvent
- customgave the crude product
- customThe crude product was purified on a silica column (1-4% MeOH/DCM)