反应详情

温度

70 °C

A portion (50 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 (373 mg) in dried dimethylformamide (20 ml). After addition of ethyl chloroacetate (123 mg), the mixture was stirred at 70° C. for one hour. The solvent was evaporated at reduced pressure, and the residue was extracted with CHCl3, and the CHCl3 extract was washed with water, dried over anhydrous MgSO4 and concentrated. The residue was recrystallized from ethanol to give 3-(2-chlorophenyl)-1-ethoxycarbonylmethyl-6-ethoxycarbonyl-5,7-dimethyl-2,4(1H,3H)-quinazolinedione (287 mg, 62.6%) melting at 158°-159° C. MS: m/e, 458(M+), 423. NMR: δ (ppm, CDCl3), 1.28 (3H, t), 1.39 (3H, t), 2.40 (3H, s), 2.74 (3H, s), 4.28 (2H, q), 4.42 (2H, q), 4.92 (2H, s), 6.74 (1H, s), 7.41 (4H, m).

1. customThe solvent was evaporated at reduced pressure
2. extractionthe residue was extracted with CHCl3
3. extractionthe CHCl3 extract
4. washwas washed with water
5. dry with materialdried over anhydrous MgSO4
6. concentrationconcentrated
7. customThe residue was recrystallized from ethanol