反应详情

温度

100 °C

A 2-liter round bottom flask was charged with 7-(benzyloxy)-3-nitroquinolin-4-ol (100.0 g, 0.3 mol) and N,N-dimethylformamide (DMF) (650 mL). Phosphorous oxychloride (62.1 g, 37.7 mL, 1.2 equivalents (eq)) was slowly added dropwise. The resulting mixture was heated at 100° C. for 10 minutes, and then allowed to cool to 39° C. The reaction mixture was poured over ice (3 L). A brown precipitate formed. The mixture was diluted with water (1 L) and stirred to break up the precipitate. The precipitate was collected by vacuum filtration. The filter cake was washed with water (2 L) and air-dried on vacuum filter for 1 hour. The solid was dissolved in dichloromethane and placed in a separatory funnel. The water was removed, and the dichloromethane solution was dried over magnesium sulfate. The solution was then filtered through filter agent to provide a solution of 7-(benzyloxy)-4-chloro-3-nitroquinoline in dichloromethane (approximately 1700 mL).

1. temperatureto cool to 39° C
2. customA brown precipitate formed
3. filtrationThe precipitate was collected by vacuum filtration
4. washThe filter cake was washed with water (2 L)
5. customair-dried on vacuum
6. filtrationfilter for 1 hour
7. dissolutionThe solid was dissolved in dichloromethane
8. customplaced in a separatory funnel
9. customThe water was removed
10. dry with materialthe dichloromethane solution was dried over magnesium sulfate
11. filtrationThe solution was then filtered
12. filtrationthrough filter agent