反应详情

温度

100 °C

To the dry N,N-dimethylformamide (45 ml) and 1-(4-hydroxyphenyl)urea (15 g, 0.0985 mol) solution were added triethylamine (34 ml, 0.24646 mol) and 3-trifluoromethyl-4-chloroaniline (19.28 g, 0.0985 mol) in one lot. This reaction mass was then agitated at 100° C. for 10-12 hours, quenched in water and the aqueous layer was extracted with ethyl acetate. The ethyl acetate layer was back washed with water and dried over sodium sulfate. It was evaporated under vacuum to obtain solid. The obtained solid was slurried in acetonitrile (100 ml) at ambient temperature, filtered and washed repeatedly with acetonitrile till the clear filtrate was obtained. The obtained cake was then suck dried for 10 minutes and vacuum dried at 50° C. to give 1-(4-chloro-3-(trifluoromethyl)phenyl)-3-(4-hydroxyphenyl)urea (25 g).

1. customquenched in water
2. extractionthe aqueous layer was extracted with ethyl acetate
3. washThe ethyl acetate layer was back washed with water
4. dry with materialdried over sodium sulfate
5. customIt was evaporated under vacuum
6. customto obtain solid
7. filtrationfiltered
8. washwashed repeatedly with acetonitrile till the clear filtrate
9. customwas obtained
10. customThe obtained cake was then suck dried for 10 minutes
11. customvacuum dried at 50° C.