反应详情

温度

80 °C

To the solution of 2-amino-3-{[2-methyl-3-(trifluoromethyl)phenyl]methyl}pyrazolo[1,5-a]pyrimidine-5,7(4H,6H)-dione (1.5 g, 4.43 mmol) in acetonitrile (100 mL) was added phthalic anhydride (1.511 g, 10.20 mmol). The reaction mixture was stirred at 80° C. for 4 days. The reaction was concentrated. To the crude was added DCM (20 mL). The insoluble solid was filtered which is the pure product. The filtrate was purified on a silica column (eluting with 20-60% EtOAc/Hexane) which was combined with the solid from filtration to give the product (1.0 g, 48%). 1H NMR (400 MHz, DMSO-d6) δ ppm 2.20 (s, 3H) 3.93 (br. s., 2H) 6.89 (t, J=7.83 Hz, 1H) 7.10 (m, 1H) 7.22 (m, 1H) 7.49-7.62 (m, 1H) 7.62-7.70 (m, 1H) 7.79-7.94 (m, 4H); LC/MS: MS (ES+) m/e 469.1 [M+H]+.

1. concentrationThe reaction was concentrated
2. additionTo the crude was added DCM (20 mL)
3. filtrationThe insoluble solid was filtered which
4. customThe filtrate was purified on a silica column (eluting with 20-60% EtOAc/Hexane) which
5. filtrationwas combined with the solid from filtration