反应详情

温度

100 °C

A mixture of 1-(3-phenylbenzofuran-2-yl)ethylamine Example 24 (0.706 mmol), 6-chloro-9H-purine (213 mg, 1.38 mmol) and DIPEA (0.24 mL, 1.38 mmol) in n-butanol (5 mL) was heated at 100° C. for 18 h. After cooling to RT, volatiles were removed under reduced pressure and the resulting residue was purified by column chromatography (Si—PCC, gradient 0-5% MeOH in DCM) and then triturated from MeOH with water affording 103 as an off-white solid (107 mg, 43% over two steps). LCMS: RT 4.15 min [M+H]+ 356.1. 1H NMR (DMSO, 400 MHz): δ 8.21-7.95 (3H, m), 7.73-7.60 (3H, m), 7.58-7.49 (3H, m), 7.46-7.23 (3H, m), 5.84 (1H, s), 1.67 (3H, d, J=6.99 Hz)

1. temperatureAfter cooling to RT
2. customvolatiles were removed under reduced pressure
3. customthe resulting residue was purified by column chromatography (Si—PCC, gradient 0-5% MeOH in DCM)
4. customtriturated from MeOH with water affording 103 as an off-white solid (107 mg, 43% over two steps)