反应详情

A suspension of 6-methoxy-2H-phthalazin-1-one (6.4 g, 36.3 mmoles), prepared as described in example 3, in acetonitrile (65 ml) under stirring and dry N2 at room temperature, was dropwise added with phosphorous oxychloride (6.8 ml, 73 mmoles), then the mixture was refluxed. After 3 hours the mixture was concentrated, taken up in water, neutralised with NaHCO3 and extracted more times with CH2Cl2. The organic phases were washed with water, anhydrified and concentrated to give 6.94 g of the title compound (yield: 98.3%). m.p.: 181-183° C.

1. customprepared
2. temperaturethe mixture was refluxed
3. concentrationAfter 3 hours the mixture was concentrated
4. extractionextracted more times with CH2Cl2
5. washThe organic phases were washed with water, anhydrified
6. concentrationconcentrated