反应详情

温度

30 °C

25.9 g (0.1 mol) of N-[2-(4-nitrophenylamino)ethyl]methanesulfonamide (22) were dissolved in 200 mL of 1N sodium hydroxide at 50° C. The insoluble matter was filtered off, the filtrate was cooled to 30° C. and 11.4 mL (0.12 mol) of methyl sulfate were added dropwise. The mixture was stirred for 1 hour at room temperature and then heated to 40° C. and the yellow precipitate was filtered off. The product was reslurried in 0.5N sodium hydroxide and in water. The wet crude product was recrystallized from 50 mL of 96% ethanol with carbon black. 13.3 g of product with a melting point of 109° C. were isolated.

1. filtrationThe insoluble matter was filtered off
2. temperatureheated to 40° C.
3. filtrationthe yellow precipitate was filtered off
4. customThe wet crude product was recrystallized from 50 mL of 96% ethanol with carbon black