反应详情

To a solution of (R)—N-(1-benzylpiperidin-3-yl)-N-methyl-7-tosyl-7H-pyrrolo[2,3-d]pyrimidin-4-amine (750 mg, 1.5 mmol) in MeOH under nitrogen, 10% Pd/C (750 mg) was added. To this suspension, ammonium formate (995 mg, 15 mmol) was added and the reaction mixture was refluxed under nitrogen for 2 h. After completion of the reaction (TLC), the reaction mixture was cooled to rt and filtered over celite. The filtrate was concentrated in vacuo to give a residue, that was purified by column chromatography (silica gel, gradient EtOAc in hexanes) to afford the titled intermediate (395 mg, 65%). 1H NMR (400 MHz, DMSO-d6): δ 8.27 (s, 1H), 7.97 (d, J=7.6 Hz, 2H), 7.65 (d, J=2.8 Hz, 1H), 7.43 (d, J=8.0 Hz, 2H), 7.01 (d, J=3.2 Hz, 1H), 5.03 (bs, 1H), 3.10-2.95 (m, 3H), 2.82-2.76 (m, 2H), 2.50 (s, 3H), 2.36 (s, 3H), 1.89-1.75 (m, 4H). LC-MS: m/z [M+1]=386.

1. temperaturethe reaction mixture was refluxed under nitrogen for 2 h
2. customAfter completion of the reaction (TLC)
3. filtrationfiltered over celite
4. concentrationThe filtrate was concentrated in vacuo
5. customto give a residue, that
6. customwas purified by column chromatography (silica gel, gradient EtOAc in hexanes)