(4-hydroxyphenyl)urea

反応条件: temp:100.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 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). quenched in water the aqueous layer was extracted with ethyl acetate The ethyl acetate layer was back washed with water dried over sodium sulfate It was evaporated under vacuum to obtain solid filtered washed repeatedly with acetonitrile till the clear filtrate was obtained The obtained cake was then suck dried for 10 minutes vacuum dried at 50° C.

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 4-aminophenol (45 g, 0.4123 mol) was charged in water and acetic acid mixture (9:1) (450 vol) to obtain a clear solution. To this clear solution was added drop wise previously prepared solution of sodium cyanate (29.48 g, 0.45358 mol) in water over a period of 1 hour. The reaction mass obtained was stirred for 6 hours at ambient temperature and filtered to obtain solid. The solid was washed with water and vacuum dried to obtain the desired product, i.e., 1-(4-hydroxyphenyl)urea (48 g). The reaction mass obtained filtered to obtain solid The solid was washed with water and vacuum dried