反应详情

温度

0 °C

24 ml of triethylamine were added over 5 minutes to a stirred mixture of 15 g of N-methylhydroxylamine hydrochloride in 100 ml of chloroform cooled to 0° C and then 37.5g of 3-trifluoromethyl-4-nitrophenyl isocyanate were added at 20° to 25° C. The mixture was stirred at 20° C for 16 hours and was then poured into water. The mixture was vacuum filtered and the recovered crystals were dried under reduced pressure. The raw product was taken up in hot isopropyl ether and the solution was treated with activated carbon and was evaporated to dryness under reduced pressure to obtain 20 g of N-hydroxy-N-methyl-N'-(3'-trifluoromethyl-4'-nitrophenyl)-urea melting at 129°-130° C.

1. filtrationfiltered
2. customthe recovered crystals were dried under reduced pressure
3. additionthe solution was treated with activated carbon
4. customwas evaporated to dryness under reduced pressure