反应详情

A stirred solution of 3,5-dimethyl-pyridyl-4-carbaldehyde (2.3 g, Reference Example 24) in methylated spirit (50 ml), at room temperature and under nitrogen, was treated with powdered sodium borohydride (1.28 g). After stirring for 6 hours the resulting homogeneous solution was allowed to stand at room temperature for a further 12 hours then treated with water (10 ml). The reaction mixture was evaporated, then azeotroped with toluene. The residue was extracted three times with hot dichloromethane (100 ml). The combined extracts were evaporated to afford a white solid which was subjected to flash chromatography on silica, eluting with a mixture of ethyl acetate and pentane (1:1, v/v) to afford the title compound (1.2 g) as a white solid, map. 93-95° C.

1. waitto stand at room temperature for a further 12 hours
2. customThe reaction mixture was evaporated
3. customazeotroped with toluene
4. extractionThe residue was extracted three times with hot dichloromethane (100 ml)
5. customThe combined extracts were evaporated
6. customto afford a white solid which
7. washeluting with a mixture of ethyl acetate and pentane (1:1