反应详情

温度

10 °C

3. 63.5 g of 4-chloro-2-(chloromethyl)-6-methylquinazoline are dissolved in 630 ml of absolute tetrahydrofuran at room temperature and then cooled to 10° C. 27.2 ml of hydrazine hydrate are added dropwise thereto within 8 min., whereby a solution results and the temperature rises to 15° C. The reaction mixture is stirred at 5° to 15° C. for 4 h. and then poured into a solution of 40 g of sodium hydrogen carbonate in 5 l of water. The mixture is extracted five times with 1.5 l of dichloromethane each time. The combined organic phases are washed with water, dried and concentrated (T<40° C.) in a vacuum to a volume of 0.5 l. 0.5 l of ethyl acetate is added thereto and the dichloromethane is evaporated completely in a vacuum, whereby the product crystallizes out. The mixture is left to stand at -25° C. overnight and the crystals are filtered off, washed with diethyl ether and dried at room temperature in a vacuum. There are obtained 38 g of 2-(chloromethyl)-4-hydrazino-6-methylquinazoline of m.p. above 140° C. (dec.).

1. customwhereby a solution results
2. customrises to 15° C
3. extractionThe mixture is extracted five times with 1.5 l of dichloromethane each time
4. washThe combined organic phases are washed with water
5. customdried
6. concentrationconcentrated (T<40° C.) in a vacuum to a volume of 0.5 l
7. addition0.5 l of ethyl acetate is added
8. customthe dichloromethane is evaporated completely in a vacuum, whereby the product
9. customcrystallizes out
10. waitThe mixture is left
11. waitto stand at -25° C. overnight
12. filtrationthe crystals are filtered off
13. washwashed with diethyl ether
14. customdried at room temperature in a vacuum