反应详情

温度

80 °C

2,6-Dichloro-N4-cyclobutylpyrimidine-4,5-diamine (crude, 5.65 mmol) in diethoxymethyl acetate (8 mL) was stirred and heated at 80° C. for 16 hr. The mixture was cooled to rt, diluted with EtOAc (80 mL) and washed with water (80 mL), sat. NaHCO3 (80 mL) and brine (80 mL). The organic layer was dried over Na2SO4 and concentrated. The crude product was purified via flash chromatography eluting with 20-50% EtOAc/heptanes to give the title compound as an off-white solid (727 mg, 53% yield). 1H NMR (400 MHz, DMSO-d6) δ ppm 8.95 (1 H, s) 5.07 (1 H, quin, J=8.56 Hz) 2.59-2.77 (2 H, m) 2.42-2.50 (2 H, m) 1.71-1.96 (2 H, m); m/z (APCI+) for C9H8Cl2N4 243.10 (M+H)+.

1. temperatureThe mixture was cooled to rt
2. washwashed with water (80 mL), sat. NaHCO3 (80 mL) and brine (80 mL)
3. dry with materialThe organic layer was dried over Na2SO4
4. concentrationconcentrated
5. customThe crude product was purified via flash chromatography
6. washeluting with 20-50% EtOAc/heptanes