反应详情

温度

100 °C

4. 58.2 g of 2-(chloromethyl)-4-hydrazino-6-methylquinazoline in 870 ml of triethyl orthoformate are heated to reflux temperature while stirring in an oil bath pre-heated to 100° C. and stirred at this temperature for a further 0.5 h. (bath temperature 140°-145° C.). About 40 ml of ethanol are distilled off during the heating. Thereafter, the mixture is concentrated in a vacuum to a volume of about 150 ml. 150 ml of diethyl ether are then added thereto, the mixture is cooled to 0° to 5° C. and the crystals are filtered off. The product is washed with ethanol/diethyl ether 1:2 and with diethyl ether and dried in a vacuum. 55.1 g of crude 5-(chloro-methyl)-9-methyl-1,2,4-triazolo[4,3-c]quinazoline of m.p. 175° C. are obtained.

1. temperatureto reflux temperature
2. stirringstirred at this temperature for a further 0.5 h. (bath temperature 140°-145° C.)
3. distillationAbout 40 ml of ethanol are distilled off during the heating
4. concentrationThereafter, the mixture is concentrated in a vacuum to a volume of about 150 ml
5. addition150 ml of diethyl ether are then added
6. temperaturethe mixture is cooled to 0° to 5° C.
7. filtrationthe crystals are filtered off
8. washThe product is washed with ethanol/diethyl ether 1:2 and with diethyl ether
9. customdried in a vacuum