反应详情

温度

100 °C

2,6-Dichloro-9-isopropyl-9H-purine (1.16 g, 5 mmol), as prepared in step 1 of Example 1, was mixed with 4-amino-1-methylpyrazole (1.02 g, 10 mmol) and DIPEA (1.74 mL, 10 mmol) in nBuOH (33 mL) and was stirred and heated at 100° C. (block temperature) for 1 hr. The reaction was cooled, and the volatiles were removed under vacuum to give a dark residue. Ethyl acetate (120 mL) was added and the mixture was washed with sat. aq. NaHCO3 (3×30 mL), dried over Na2SO4 and evaporated to give a dark residue. This residue was dissolved in ethyl acetate, passed through a thin pad of silica gel, and eluted with 90% ethyl acetate-10% ammonia (7 N in methanol). The eluent was evaporated to afford the title compound as a dark solid (1.43 g, 98% yield). 1H NMR (400 MHz, DMSO-d6) δ ppm 10.41 (br. s., 1 H) 8.38 (s, 1 H) 8.00 (s, 1 H) 7.68 (s, 1 H) 4.71 (quin, J=6.72 Hz, 1 H) 3.84 (s, 3 H) 1.52 (d, J=6.72 Hz, 6 H). m/z (APCI+) for C12H14ClN7 292.1 with Cl isotope pattern (M+H)+.

1. temperatureThe reaction was cooled
2. customthe volatiles were removed under vacuum
3. customto give a dark residue
4. washthe mixture was washed with sat. aq. NaHCO3 (3×30 mL)
5. dry with materialdried over Na2SO4
6. customevaporated
7. customto give a dark residue
8. washeluted with 90% ethyl acetate-10% ammonia (7 N in methanol)
9. customThe eluent was evaporated