反应详情

To a solution of 5.39 g of 4-(m-chlorophenyl)-imidazo[1,5-a]pyrimidine-8-carboxamide (Example 14) in 100 ml of glacial acetic acid, was added in portions 2.8 g of sodium cyanoborohydride at room temperature under nitrogen. The mixture stirred at room temperature for 2 hours. The solvent was evaporated in vacuo to give an oil, and this was dissolved in dichloromethane, then washed with saturated sodium bicarbonate solution, The organic layer was separated, dried over anhydrous sodium sulfate and filtered through a short column of hydrous magnesium silicate. Evaporation of the solvent gave a yellow solid which was recrystallized from acetonitrile to give 3.25 g of the desired product as a yellow solid, mp 182°-184° C.

1. customThe solvent was evaporated in vacuo
2. customto give an oil
3. washwashed with saturated sodium bicarbonate solution
4. customThe organic layer was separated
5. dry with materialdried over anhydrous sodium sulfate
6. filtrationfiltered through a short column of hydrous magnesium silicate
7. customEvaporation of the solvent
8. customgave a yellow solid which
9. customwas recrystallized from acetonitrile