反应详情

To a solution of 5-chloroisatoic anhydride (10.0 g, 51 mmol) in tetrahydrofuran (100 ml) at ambient temperature was added a 40% w/w aqueous solution of methylamine (19.80 g, 255 mmol) dropwise. The mixture was stirred at an ambient temperature for 1 hour. Ethyl acetate (100 ml) and water (100 ml) were added and the phases separated. The aqueous layer was back extracted with ethyl acetate (100 ml) and the combined organics were evaporated under reduced pressure to afford a white solid, which was recrystallised from toluene (60 ml) to afford the title compound as a white solid (8.15 g)

1. customthe phases separated
2. extractionThe aqueous layer was back extracted with ethyl acetate (100 ml)
3. customthe combined organics were evaporated under reduced pressure
4. customto afford a white solid, which
5. customwas recrystallised from toluene (60 ml)