反应详情

温度

10 °C

1. 91.4 g of methyl 2-amino-5-methylbenzoate and 23.4 ml of chloroacetonitrile are dissolved in 1.01 of absolute dioxan and the solution is cooled to 10° C. Subsequently, a weak stream of dry hydrogen chloride is introduced for 8 h. at 5° to 15° C. After 4 h., a further 23.4 ml of chloroacetonitrile are added thereto. The mixture is stirred at room temperature for a further 18 h. The suspension is subsequently evaporated in a vacuum. The crystalline residue is suspended with 2.51 of ice/water, adjusted to pH 8 to 9 with about 100 ml of 25% ammonia, stirred at 5° C. for 1 h. and then filtered. The crystals are washed with water and dried in a vacuum. There are obtained 114.1 g of 2-chloromethyl-6-methyl-3H-quinazolin-4-one of m.p. 263°-265° C.

1. customThe suspension is subsequently evaporated in a vacuum
2. stirringstirred at 5° C. for 1 h.
3. filtrationfiltered
4. washThe crystals are washed with water
5. customdried in a vacuum