HRID475244
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 25 °C
PROCEDURE
实验过程
A mixture of 162 (9.8 g, 52.5 mmol), MeOH(NH3 in MeOH) and Raney-Ni (>15 eq) was stirred under hydrogen at 25° C. for 2 h. The mixture was filtered and concentrated in vacuo. The crude product was purified by SiO2 chromatography eluting with a MeOH/DCM gradient (0% to 10% MeOH) to afford 7.0 g (70%) of (4-methyl-1-tetrahydropyran-2-yl-benzimidazol-5-yl)methanamine (164) as yellowish oil: LC/MS: m/z=246 [M+1]+.
WORKUP
后处理
- filtrationThe mixture was filtered
- concentrationconcentrated in vacuo
- customThe crude product was purified by SiO2 chromatography
- washeluting with a MeOH/DCM gradient (0% to 10% MeOH)