反应详情

温度

60 °C

A suspension of 0.45 g 7-bromo-2-methyl-3H-quinazolin-4-one in 0.48 ml N,N-dimethylaniline is treated with 1.41 ml phosphourous oxychloride and heated at 60° C. for 2 h. The reaction mixture is evaporated in vacuo and the residue is taken up with 20 ml water, neutralized with 10 ml saturated aqueous sodium bicarbonate and extracted with 25 ml dichloromethane twice. The organic layer is washed with 25 ml water, 25 ml brine, dried over magnesium sulfate and evaporated in vacuo. The residue is purified by chromatography on silica gel with Heptane/ethylacetate 2:1. 0.288 g (59%) of 7-bromo-4-chloro-2-methyl-quinazoline are obtained as an orange solid. Mp. >82° C. (dec). MS (EI): peaks at m/e: 258(M+, 37%), 221 (100%), 179(9%).

1. customThe reaction mixture is evaporated in vacuo
2. extractionextracted with 25 ml dichloromethane twice
3. washThe organic layer is washed with 25 ml water, 25 ml brine
4. dry with materialdried over magnesium sulfate
5. customevaporated in vacuo
6. customThe residue is purified by chromatography on silica gel with Heptane/ethylacetate 2:1