反应详情

To a solution of 2-N-methyl-2-N-phenyl-6-{5-[(2S)-pyrrolidin-2-yl]-1,2,4-oxadiazol-3-yl}-1,3,5-triazine-2,4-diamine hydrochloride (Example 438, 0.2 g, 0.535 mmol) in DCE (5 mL) was added sodium acetate (0.07 g, 0.8 mmol) and 3,3,3-trifluoropropanal (0.12 g, 1.070 mmol) and the mixture was stirred for 1 h at room temperature. Sodium triacetoxyborohydride (0.17 g, 0.8 mmol) was added and the reaction mixture was stirred for 2 h at room temperature. DCM was added and the mixture was washed with saturated aq. sodium bicarbonate, and then brine. The organic layer was dried over sodium sulfate and concentrated under vacuum. The residue was purified by FCC, eluting with 20-100% EtOAc in heptane to afford the title compound (0.045 g, 19%).

1. stirringthe reaction mixture was stirred for 2 h at room temperature
2. washthe mixture was washed with saturated aq. sodium bicarbonate
3. dry with materialThe organic layer was dried over sodium sulfate
4. concentrationconcentrated under vacuum
5. customThe residue was purified by FCC
6. washeluting with 20-100% EtOAc in heptane