反应详情

Phosphorous oxychloride (19.5 mL, 210 mmol) and 8-iodo-7-methylquinazolin-4(3H)-one (2.00 g, 6.99 mmol) were added to a round bottomed flask. The reaction mixture was heated at reflux for 2 h. Upon cooling, excess POCl3 was removed under reduced pressure and the remaining crude product dissolved in DCM (100 mL) and washed with ice-cold water (300 mL) to remove excess acid. The crude residue dissolved in DCM was then dried over anhydrous sodium sulfate and concentrated in vacuo to give 4-chloro-8-iodo-7-methylquinazoline (1.96 g, 92%) as an amorphous brown solid. MS (M+H)+ 305.

1. temperatureThe reaction mixture was heated
2. temperatureat reflux for 2 h
3. temperatureUpon cooling
4. customexcess POCl3 was removed under reduced pressure
5. dissolutionthe remaining crude product dissolved in DCM (100 mL)
6. washwashed with ice-cold water (300 mL)
7. customto remove excess acid
8. dissolutionThe crude residue dissolved in DCM
9. dry with materialwas then dried over anhydrous sodium sulfate
10. concentrationconcentrated in vacuo