反应详情

Under a nitrogen atmosphere, a suspension of N1-(3-nitroquinolin-1-yl)-2-methylpropane-1,2-diamine (60.0 g, 231 mmol) in dichloromethane (1.0 L) was chilled in an ice bath. Isopropyl isocyanate (23.8 mL, 242 mmol) was added dropwise over a period of 10 minutes. The reaction was allowed to slowly warm to room temperature. After 17 hours additional isopropyl isocyanate (about 2 mL) was added. After an additional 3 hours more isopropyl isocyanate (1 mL) was added. After 2 more hours the reaction mixture was concentrated under reduced pressure to provide 79.8 g of 1-{1,1-dimethyl-2-[(3-nitroquinolin-1-yl)amino]ethyl}-3-(1-methylethyl)urea as a bright yellow solid.

1. temperaturewas chilled in an ice bath
2. concentrationAfter 2 more hours the reaction mixture was concentrated under reduced pressure