反应详情

温度

130 °C

A mixture of phosphorous oxychloride (5 mL) and 6-bromo-7-methyl-8-nitroquinazolin-4(3H)-one (800 mg, 2.82 mmol) was refluxed at 130° C. for 4 h. On cooling, POCl3 was removed under reduced pressure. The resulting crude product residue was diluted with ice-water and extracted out of the aqueous layer with DCM (3×20 mL). The combined organic extracts were dried over anhydrous sodium sulfate and concentrated to give 6-bromo-4-chloro-7-methyl-8-nitroquinazoline (595 mg, 70% yield) as an amorphous light yellow solid. MS (ESI, pos. ion) m/z: 302 [M+H]+

1. temperatureOn cooling
2. customPOCl3 was removed under reduced pressure
3. additionThe resulting crude product residue was diluted with ice-water
4. extractionextracted out of the aqueous layer with DCM (3×20 mL)
5. dry with materialThe combined organic extracts were dried over anhydrous sodium sulfate
6. concentrationconcentrated