反应详情

温度

120 °C

A mixture of (S)-2-(1-aminoethyl)-1-cyclopropyl-N-methyl-1H-benzo[d]imidazole-7-carboxamide (Prepared in Example 20, 190 mg, 0.74 mmol), 6-chloro-5-iodopyrimidin-4-amine (188 mg, 0.736 mmol) and 1,1′-dimethyltriethylamine (256 μL, 1.47 mmol) in n-butanol (2 mL) was stirred at 120° C. After 18 h, the mixture was cooled to rt and concentrated under reduced pressure. The residue was purified by column chromatography on a silica gel column using 0 to 10% gradient of MeOH in DCM-EtOAc (1:1) as eluent to give (S)-2-(1-(6-amino-5-iodopyrimidin-4-ylamino)ethyl)-1-cyclopropyl-N-methyl-1H-benzo-[d]imidazole-7-carboxamide: 1H NMR (400 MHz, DMSO-d6) δ 8.46-8.40 (m, 1H), 7.87 (s, 1H), 7.67 (d, J=8 Hz, 1H), 7.24 (d, J=8 Hz, 1H), 7.20 (dd, J=8, 8 Hz, 1H), 6.46 (m, 1H), 6.37 (d, J=8 Hz, 1H), 5.82-5.75 (m, 1H), 2.84 (d, J=4 Hz, 3H), 1.60 (d, J=8 Hz, 3H), 1.14-1.04 (m, 2H), 0.93-0.90 (m, 1H), 0.85-0.76 (m, 1H); LC-MS (ESI) m/z 478.0 [M+H]+.

1. temperaturethe mixture was cooled to rt
2. concentrationconcentrated under reduced pressure
3. customThe residue was purified by column chromatography on a silica gel column