反应详情

A solution of 5-butyl-N-(2,4-dimethoxybenzyl)-3-(6-(pyrrolidin-1-yl)hex-1-yn-1-yl)-1H-pyrazolo[4,3-d]pyrimidin-7-amine (20 g, 40.8 mmol) in ethanol (500 mL) was hydrogenated over Pd—C (5 g, 4.70 mmol) for 4 hour (H2 uptake complete). The mixture was filtered through Hyflo and evaporated. The residue in DCM (30 mL) was purified on a 120 g silica cartridge (Redisep Gold) eluted with toluene-ethanol-NH3 (85/15/1.5) in 7 batches-taking off product and lower running impurity and recycling the cartridge each time (total volume˜3 liters). Evaporation of appropriate fractions gave the title compound as a yellow gum (16.3 g).

1. filtrationThe mixture was filtered through Hyflo
2. customevaporated
3. customThe residue in DCM (30 mL) was purified on a 120 g silica cartridge (Redisep Gold)
4. washeluted with toluene-ethanol-NH3 (85/15/1.5) in 7 batches-taking off product
5. customEvaporation of appropriate fractions