反应详情

To a solution of (1R,3S)-3-isopropyl-3-(4-[6-(trifluoromethyl)pyridin-2-yl]piperazin-1-ylcarbonyl)cyclopentanamine dihydrochloride (120 mg, 0.26 mmol), 3-methyltetrahydro-4H-pyran-4-one (75 mg, 0.66 mmol), triethylamine (0.15 mL, 1.0 mmol) in methylene chloride (8 mL) was added sodium triacetoxyborohydride (0.17 g, 0.79 mmol). After being stirred at room temperature overnight, the reaction mixture was diluted with water and extracted with ethyl acetate three times, dried with sodium sulfate, filtered, and concentrated in vacuo. The crude residue was purified by flash column chromatography (ethyl acetate to EtOAc/Et3N=10:0.1) to yield the desired product (100 mg, 79%). LCMS calculated for C25H38F3N4O2: (M+1) 483.2; found 483.2.

1. extractionextracted with ethyl acetate three times
2. dry with materialdried with sodium sulfate
3. filtrationfiltered
4. concentrationconcentrated in vacuo
5. customThe crude residue was purified by flash column chromatography (ethyl acetate to EtOAc/Et3N=10:0.1)