反应详情

温度

120 °C

A mixture of 318 mg (1 mmol) of N-(6-fluoro-7-nitro-2,4-dioxo-1,4-dihydro-2H-quinazolin-3-yl)-methanesulfonamide, 605 mg (4.0 mmol) of 2-benzyloxy-ethylamine and 3.2 ml of ethanol is heated at 120° C. in a closed vial in a microwave reactor for 10 minutes. After cooling to room temperature, 1M aqueous hydrochloric acid is added until a pH value of ˜3 is reached. The resulting mixture is extracted with ethyl acetate. The organic phase is separated, washed with water and brine, dried over magnesium sulfate and evaporated. Chromatography of the residue on silica with dichloro-methane-methanol (93:7) and crystallization from tetrahydrofuran-hexane gives 261 mg (58%) of the title compound as red crystals, m.p. 204° C. (decomp.).

1. temperatureAfter cooling to room temperature
2. extractionThe resulting mixture is extracted with ethyl acetate
3. customThe organic phase is separated
4. washwashed with water and brine
5. dry with materialdried over magnesium sulfate
6. customevaporated
7. customChromatography of the residue on silica with dichloro-methane-methanol (93:7) and crystallization from tetrahydrofuran-hexane