反应详情

温度

100 °C

A mixture of (S)—N-[4-fluoro-2-(6-fluoropyridin-3-ylamino)phenyl]-2-(9H-purin-6-ylamino)propionamide (255 mg, 0.62 mmol) in AcOH (10 mL) was heated at 100° C. for 24 h. After cooling to RT, the volatiles were removed under reduced pressure and the residue was partitioned between EtOAc and a saturated aqueous solution of NaHCO3. The aqueous phase was extracted with EtOAc and the combined organic fractions washed with water, followed by brine, dried (Na2SO4) and concentrated in vacuo. The resulting residue was purified by column chromatography (Si—PCC, gradient 0-20% 2M NH3/MeOH in DCM) to afford 382 as a pink solid (38 mg, 16%). LCMS (Method K): RT 2.40 min [M+H]+ 391.0. 1H NMR (DMSO-d6+TFA-D, 400 MHz, 80° C.): δ 8.58-8.49 (2H, m), 7.82 (1H, d, J=2.96 Hz), 7.75 (1H, dd, J=8.81, 4.70 Hz), 7.51 (1H, dd, J=9.59, 2.99 Hz), 7.21-7.07 (2H, m), 6.40 (1H, d, J=9.60 Hz), 5.86 (1H, br d), 1.79 (3H, d, J=6.82 Hz)

1. temperatureAfter cooling to RT
2. customthe volatiles were removed under reduced pressure
3. customthe residue was partitioned between EtOAc
4. extractionThe aqueous phase was extracted with EtOAc
5. washthe combined organic fractions washed with water
6. dry with materialdried (Na2SO4)
7. concentrationconcentrated in vacuo
8. customThe resulting residue was purified by column chromatography (Si—PCC, gradient 0-20% 2M NH3/MeOH in DCM)