反应详情

温度

25 °C

Into a 10-mL round-bottom flask, was placed cyclopropanecarbaldehyde (28.7 mg, 0.41 mmol, 2.00 equiv), piperidine (17.4 mg, 0.20 mmol, 1.00 equiv), 3-[(2R)-2-([4-amino-3-[4-(3,5-difluorophenoxy)phenyl]-1H-pyrazolo[3,4-d]pyrimidin-1-yl]methyl)pyrrolidin-1-yl]-3-oxopropanenitrile (100 mg, 0.20 mmol, 1.00 equiv), and methanol (5 mL). The resulting solution was stirred for 12 h at 25° C. and then concentrated under vacuum. The residue was loaded onto a silica gel column and eluted with dichloromethane/methanol (50/1) to give 53.12 mg (45%) of the title compound as an off-white solid. LC-MS: (ES, m/z): MS (ESI, pos. ion) m/z: 541 (M+1). H-NMR: (CDCl3, ppm): 1HNMR (300 MHz, CD3OD, ppm), 8.28 3 (1H, s), 7.777˜7.806 (2H, t), 7.269˜7.298 (2H, t), 6.703˜6.754 (3H, t), 6.455˜6.600 (1H, d), 4.400˜4.878 (3H, m), 3.338˜3.618 (2H, m), 1.700˜2.188 (4H, m), 1.280˜1.305 (4H, m), 0.710˜0.912 (2H, m).

1. customInto a 10-mL round-bottom flask, was placed
2. concentrationconcentrated under vacuum
3. washeluted with dichloromethane/methanol (50/1)