反应详情

温度

90 °C

A mixture of (S)-1-(6-fluoro-1-pyridin-2-yl-1H-benzoimidazol-2-yl)ethylamine (764 mg, 3.0 mmol), 6-chloro-9-(tetrahydropyran-2-yl)-9H-purine (710 mg, 3.0 mmol) and DIPEA (2.6 mL, 15 mmol) in IPA (8 mL) was heated for 16 h at 90° C. After cooling to RT, the volatiles were removed under reduced pressure and the resulting residue loaded onto an Isolute® SCX-2 cartridge. The cartridge was washed with MeOH followed by 2M NH3/MeOH. The basic fractions were combined, concentrated in vacuo and the resulting residue purified by column chromatography (Si—PCC, gradient 0-10% 2M NH3/MeOH in EtOAc) to afford 210 as a white solid (700 mg, 63%). LCMS (Method K): RT 2.94 min [M+H]+ 375.0. 1H NMR (DMSO-d6, 400 MHz): δ 12.89 (1H, br s), 8.61 (1H, br s), 8.20-7.80 (4H, m), 7.79-7.67 (2H, m), 7.52-7.43 (1H, m), 7.20-7.08 (2H, m), 5.86 (1H, br s), 1.63 (3H, d, J=6.82 Hz)

1. temperatureAfter cooling to RT
2. customthe volatiles were removed under reduced pressure
3. washThe cartridge was washed with MeOH
4. concentrationconcentrated in vacuo
5. customthe resulting residue purified by column chromatography (Si—PCC, gradient 0-10% 2M NH3/MeOH in EtOAc)