反应详情

A mixture of 6,7-dimethoxy-2-methylquinazolin-4(3H)-one (1.0 mg) and phosphorous oxychloride (20 mL) was refluxed for 3 h. The reaction mixture was attained to rt and poured into ice cold water and stirred for 10 min. The solution was extracted with chloroform (3×100 mL) and the combined CHCl3 layer was washed water, brine and dried over sodium sulfate. The solution was filtered and evaporated the solvent to give the product as a yellow color solid (1.0 g, 92%), mp 182-184° C. 1H NMR (400 MHz, CDCl3): δ 7.36 (1H, s), 7.30 (1H, s), 4.06 (6H, s), 2.81 (3H, s); LC-MS (positive ion mode): m/z 239, 241 (M+H)+.

1. temperaturewas refluxed for 3 h
2. customwas attained to rt
3. additionpoured into ice cold water
4. extractionThe solution was extracted with chloroform (3×100 mL)
5. washthe combined CHCl3 layer was washed water, brine
6. dry with materialdried over sodium sulfate
7. filtrationThe solution was filtered
8. customevaporated the solvent