反应详情

温度

80 °C

A heterogeneous mixture of 1-methylcyclobutanamine hydrochloride (Oakwood Chemical, cat #041889; 0.69 g, 5.70 mmol) (Oakwood Chemical, cat #041889), 2-chloro-8-iodo-3-methylquinazolin-4(3H)-one (700) (0.96 g, 3.0 mmol) and TEA (2.1 mL, 15.10 mmol) in 2 mL of THF in a sealed glass tube was heated in an oil bath at 80° C. for 4 h. The reaction mixture was diluted with EtOAc, washed with water followed by brine. The organic extract was concentrated and the residue was purified on a silica gel column (25-55% EtOAc in hexanes) to afford 8-iodo-3-methyl-2-((1-methyl-cyclobutyl)amino)quinazolin-4(3H)-one (0.94 g, 2.55 mmol, 85% yield) as a yellow crystalline solid. 1H NMR (400 MHz, DMSO-d6) δ ppm 8.11 (1H, dd, J=7.4, 1.4 Hz), 7.92 (1H, dd, J=7.8, 1.4 Hz), 7.03 (1H, s), 6.87 (1H, t, J=7.7 Hz), 3.40 (3H, s), 2.20-2.46 (4H, m), 1.88 (2H, m), 1.72 (3H, s). m/z (ESI, +ve) 370.1 (M+H)+).

1. washwashed with water
2. extractionThe organic extract
3. concentrationwas concentrated
4. customthe residue was purified on a silica gel column (25-55% EtOAc in hexanes)