反应详情

温度

90 °C

8-bromo-2-chloro-3-cyclopropylquinazolin-4(3H)-one (723) (213 mg, 0.711 mmol) was treated with tert-butylamine (0.90 mL, 8.56 mmol) and heated at 90° C. in a sealed tube for 24 h. The reaction mixture was concentrated to remove the excess t-BuNH2 and the crude residue was chromatographed on an ISCO Combiflash RF (12 g Redisep column, using a gradient of 0-5% MeOH in DCM) affording 8-bromo-2-(tert-butylamino)-3-cyclopropylquinazolin-4(3H)-one (224 mg, 0.66 mmol, 94% yield) as an off-white crystalline solid. 1H NMR (400 MHz, CDCl3) δ ppm 8.02 (1H, dd, J=8.0, 1.4 Hz), 7.82 (1H, dd, J=7.7, 1.5 Hz), 6.94 (1H, t, J=7.7 Hz), 5.42 (1H, s), 2.62-2.71 (1H, m), 1.61 (9H, s), 1.28-1.35 (2H, m), 0.87-0.95 (2H, m). m/z (ESI, +ve) 335.9/337.9 (M+1)+.

1. concentrationThe reaction mixture was concentrated
2. customto remove the excess t-BuNH2
3. customthe crude residue was chromatographed on an ISCO Combiflash RF (12 g Redisep column