HRID475244

反应详情

EQUATION

反应方程式

HRID 475244 反应方程式

AUXILIARIES

试剂、催化剂与溶剂

2

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

  1. filtrationThe mixture was filtered
  2. concentrationconcentrated in vacuo
  3. customThe crude product was purified by SiO2 chromatography
  4. washeluting with a MeOH/DCM gradient (0% to 10% MeOH)