反应详情

温度

110 °C

19.9 Grams (0.293 mol) of imidazole and 54.7 g (0.304 mol) of sodium methylate solution (30% in methanol) are mixed and concentrated to dryness at 50° C./12 Torr. 80 Ml of dimethylformamide are added to the thus-formed imidazole sodium salt. The mixture is heated to 110° C. and a solution of 50 g (0.197 mol) of N-(3-chloro-2-hydroxypropyl)-3,4-dichloroaniline in 100 ml of dimethylformamide is added dropwise at this temperature over a period of 30 minutes. This addition finished, the reaction solution is further heated and refluxed for 2 hours. The solution is then cooled to 90° C. and 650 ml of water are added. The reaction mixture is left standing for 12 hours. The solid precipitant is filtered off, washed with water and dried at 50° C./12 Torr. For purification the substance is recrystallized under filtration with active charcoal from 100 ml ethyl acetate to yield 22 g of 1-[3-(3,4-dichloroanilino)-2-hydroxypropyl]-imidazole, M.P. 98°-100° C.

1. concentrationconcentrated to dryness at 50° C./12 Torr
2. addition80 Ml of dimethylformamide are added to the thus-formed imidazole sodium salt
3. additionThis addition
4. temperaturethe reaction solution is further heated
5. temperaturerefluxed for 2 hours
6. temperatureThe solution is then cooled to 90° C.
7. waitThe reaction mixture is left
8. filtrationThe solid precipitant is filtered off
9. washwashed with water
10. customdried at 50° C./12 Torr
11. customFor purification the substance
12. customis recrystallized under filtration with active charcoal from 100 ml ethyl acetate