反应详情

温度

80 °C

A portion (30 mg) of sodium hydride suspension (50%) in mineral oil was added to a stirred solution of 3-(2-chlorophenyl)-6-ethoxycarbonyl-5,7-dimethyl-2,4-(1H, 3H)-quinazolinedione (187 mg) in dimethylformamide (10 ml). After addition of N,N-diethyl-chloroacetamide (80 mg), the mixture was stirred at 80° C. for 3 hours. The solvent was evaporated off at reduced pressure, and the residue was extracted with CHCl3. The CHCl3 extract was washed with water, dried over NaSO4 and concentrated. The residue was recrystallized from methanol to give 3-(2-chlorophenyl)-6-ethoxycarbonyl-5,7-dimethyl-1-(N,N-diethyl)aminocarbonylmethyl-2,4(1H, 3H)-quinazolinedione (138 mg, 57%) melting at 228°-229° C. MS: M/e, 485(M+), 450. NMR: δ (ppm, CDCl3), 1.38 (9H, m), 2.39 (3H, s), 2.72 (3H, s), 3.45 (4H, q), 4.40 (2H, q), 4.95 (2H, d), 6.75 (1H, s), 7.40 (4H, m).

1. customThe solvent was evaporated off at reduced pressure
2. extractionthe residue was extracted with CHCl3
3. extractionThe CHCl3 extract
4. washwas washed with water
5. dry with materialdried over NaSO4
6. concentrationconcentrated
7. customThe residue was recrystallized from methanol