反应详情

A mixture of the crude 1-bromo-3-(3,4-dichlorophenyl)-3-methylbutan-2-one described above (3.1 g), imidazolidine-2-thione (1.2 g), ethanol (1.02 ml) and acetic acid (8 ml) was heated under reflux for 22 hours then allowed to cool to ambient temperature. The solvents were removed in vacuo and the residue was triturated with hot ethyl acetate (80 ml). The resulting solid was collected by filtration, washed with ethyl acetate (20 ml), dried in vacuo at 50° C., then crystallised from ethanol. The resulting product was collected by filtration, washed with ethanol (5 ml) and dried in vacuo at 50° C. to give 3-[1-(3,4-dichlorophenyl)-1-methylethyl]-5,6-dihydroimidazo[2,1-b]-thiazole hydrobromide as an off-white solid (0.95 g), m.p. 266-270° C. (decomposes).

1. temperaturewas heated
2. temperatureunder reflux for 22 hours
3. customThe solvents were removed in vacuo
4. customthe residue was triturated with hot ethyl acetate (80 ml)
5. filtrationThe resulting solid was collected by filtration
6. washwashed with ethyl acetate (20 ml)
7. customdried in vacuo at 50° C.
8. customcrystallised from ethanol
9. filtrationThe resulting product was collected by filtration
10. washwashed with ethanol (5 ml)
11. customdried in vacuo at 50° C.