反应详情

温度

60 °C

A suspension of 0.45 g (1.87 mmol) of 7-bromo-2-methyl-3H-quinazolin-4-one in 0.48 ml N,N-dimethylaniline was treated with 1.41 ml (15.4 mmol) phosphorous oxychloride and heated at 60° C. for 2 h. The reaction mixture was evaporated in vacuo and the residue taken up in 20 ml water, neutralized with 10 ml saturated aqueous sodium bicarbonate and twice extracted with 25 ml dichloromethane. 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) to give 0.29 g (59%) of 7-bromo-4-chloro-2-methyl-quinazoline as an orange solid. Mp. >82° C. EI mass spectrum, m/e: 258 (M calculated for C9H6BrClN2: 258).

1. customThe reaction mixture was evaporated in vacuo
2. extractiontwice extracted with 25 ml dichloromethane
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)