反应详情

To the solution of ethyl 4-methylpiperidine-4-carboxylate hydrochloride (0.9 g, 4.35 mmol) in EtOH (10 mL) was added DIPEA (2.30 mL, 13 mmol) at rt. The resulted mixture was stirred at rt for 10 minutes followed by addition of 5-bromo-2-chloropyrimidine (0.7 g, 3.6 mmol). The mixture was heated up to 70° C. for 1 h. After completion of reaction (by TLC), solvent was evaporated and the crude residue was purified over 100-200 M silica-gel by using 1.5% EtOAc:hexane to obtain the desired product as an off white solid compound (0.90 g, 75%). 1H NMR (DMSO-d6): δ 1.17 (s, 3H), 1.21 (t, J=7.20 Hz, 3H) 1.40 (m, 2H), 2.00 (m, 2H), 3.24 (m, 2H), 4.11 (m, 2H), 4.15 (q, J=7.20 Hz, 2H), 8.43 (s, 2H). MS: 328.08 [M+H]+.

1. temperatureThe mixture was heated up to 70° C. for 1 h
2. customAfter completion of reaction (by TLC), solvent
3. customwas evaporated
4. customthe crude residue was purified over 100-200 M silica-gel