HRID475194
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 66 (1.0 g, 4.11 mmol) in MeOH (10 mL) cooled to 0° C. was added NaBH4 (300 mg, 8.23 mmol). After stirring at RT overnight, the mixture was quenched with water (3 mL) and extracted with DCM (3×50 mL). The organic layers were separated, washed with brine, dried (MgSO4), filtered and concentrated in vacuo to afford 880 mg (66%) of N-methyl-1-(1-(tetrahydro-2H-pyran-2-yl)-1H-benzo[d]imidazol-5-yl)methanamine (68) as yellow oil: MS (ESI) m/z=246.2 [M+1]+.
WORKUP
后处理
- customthe mixture was quenched with water (3 mL)
- extractionextracted with DCM (3×50 mL)
- customThe organic layers were separated
- washwashed with brine
- dry with materialdried (MgSO4)
- filtrationfiltered
- concentrationconcentrated in vacuo