反应详情

温度

20 °C

To a solution of 71.2 g of ethyl 4-nitrophenoxyethaneimidoate (0.32 mol) (compound VII) in 925 ml of acetonitrile are added slowly, at 20° C., 35 ml of 37% hydrochloric acid (0.38 mol). The reaction medium is stirred at 20° C. for 2 hours and then filtered, and the O-(4-nitrophenyl)hydroxylamine hydrochloride thus formed is dried at 30° C. in a vacuum oven. With stirring, this hydrochloride is dissolved in a mixture formed from 800 ml of dichloromethane and of a sodium hydroxide solution (16.8 g in 500 ml) and the phases are then allowed to separate by settling. The organic phase is separated out and washed with 500 ml of water. This organic phase is evaporated on a rotary evaporator and the solid obtained is then dried in a vacuum oven.

1. filtrationfiltered