反应详情

Triethylamine (30 μL), 1H-benzotriazole-1-methanol (48 mg), and sodium triacetoxyborohydride (91 mg) were added to a solution of 9-methyl-6-{6-[2-(piperidin-4-yl)ethoxy]-5-(trifluoromethyl)pyridin-3-yl}-9H-purine-2-carbonitrile monohydrochloride (100 mg) in THF (1.5 mL)-EtOH (1.5 mL), and the mixture was stirred at room temperature for 16 hours. After a saturated aqueous NaHCO3 solution and EtOAc were added to the reaction mixture, extraction thereof was performed using EtOAc, and the extract was washed with saturated brine. The organic layer was dried over MgSO4 and filtered, and the filtrate was concentrated under reduced pressure. The residue was purified by silica gel column chromatography (CHCl3:MeOH=100:0 to 80:20), whereby 9-methyl-6-{6-[2-(1-methylpiperidin-4-yl)ethoxy]-5-(trifluoromethyl)pyridin-3-yl}-9H-purine-2-carbonitrile (57 mg) was obtained as a solid.

1. washthe extract was washed with saturated brine
2. dry with materialThe organic layer was dried over MgSO4
3. filtrationfiltered
4. concentrationthe filtrate was concentrated under reduced pressure
5. customThe residue was purified by silica gel column chromatography (CHCl3:MeOH=100:0 to 80:20)