反应详情

温度

40 °C

30 g of sodium were added to a solution of 88.5 g of imidazole in 600 ml of methanol; the solvent was then evaporated off. The residue was dissolved in 300 ml of dimethylformamide and heated to 115°-120° C. To the solution so obtained was added, dropwise and under stirring, a solution of 225 g of 1-(2',4'-dichlorophenyl)-2-chloro-ethanol in 400 ml of dimethylformamide. The mixture was heated to 115°-120° C. and maintained at that temperature for 20 minutes and, after subsequent cooling to 40° C., 2500 ml of iced water were added under vigorous stirring. The product precipitated under stirring over a period of about two hours, the upper liquid was then decanted off, a further 2500 ml of water were added and, after standing, the whole was filtered. The precipitate thus obtained was dried and crystallized from toluene. 170 g of the desired product, melting at 134°-135° C., was obtained.

1. customthe solvent was then evaporated off
2. dissolutionThe residue was dissolved in 300 ml of dimethylformamide
3. temperatureheated to 115°-120° C
4. customTo the solution so obtained
5. additionwas added
6. temperatureThe mixture was heated to 115°-120° C.
7. temperaturemaintained at that temperature for 20 minutes
8. customThe product precipitated
9. stirringunder stirring over a period of about two hours
10. customthe upper liquid was then decanted off
11. additiona further 2500 ml of water were added
12. filtrationthe whole was filtered
13. customThe precipitate thus obtained
14. customwas dried
15. customcrystallized from toluene