反应详情

1-(4-chloro-3-(trifluoromethyl)phenyl)urea (100 g, 0.04191 mol), 1,8-diazabicyclo[5.4.0]undec-7-ene (9.4 ml, 0.0628 mol) and 4-amino phenol (5.48 g, 0.050 mol) were mixed with dimethyl sulfoxide (25 ml) and the reaction mass was heated to 80°-90° C. for 8-9 hours. It was then cooled to room temperature and quenched in water (150 ml). The quenched mass was extracted repeatedly with ethyl acetate and the combined ethyl acetate layer was then back washed with water. The residue was then dried over sodium sulfate and evaporated under vacuum to obtain solid. The solid thus obtained was then slurried in acetonitrile (100 ml) at ambient temperature and filtered. It was washed repeatedly with acetonitrile till clear filtrate was obtained. The obtained cake was suck dried for 10 minutes and vacuum dried at 50° C. to give 1-(4-chloro-3-(trifluoromethyl)phenyl)-3-(4-hydroxyphenyl)urea (9.8 g).

1. temperaturethe reaction mass was heated to 80°-90° C. for 8-9 hours
2. customquenched in water (150 ml)
3. extractionThe quenched mass was extracted repeatedly with ethyl acetate
4. washthe combined ethyl acetate layer was then back washed with water
5. dry with materialThe residue was then dried over sodium sulfate
6. customevaporated under vacuum
7. customto obtain solid
8. customThe solid thus obtained
9. filtrationfiltered
10. washIt was washed repeatedly with acetonitrile till clear filtrate
11. customwas obtained
12. customdried for 10 minutes
13. customvacuum dried at 50° C.