反应详情

A suspension of 5-benzyloxy-6-methoxy-2H-phthalazin-1-one (4 g, 14.17 mmoles), prepared as described in example 69, in acetonitrile (40 ml), and POCl3 (6.5 ml, 70.8 mmoles) was heated at 80° C. under stirring up to dissolution. After 30 minutes the solution was evaporated and the residue taken up in CH2Cl2 (100 ml), washed with a cold solution of NaOH (20 ml) and water (200 ml) and extracted in ethyl ether (twice) and ethyl acetate (once) checking the pH to be around 7. The organic phase was washed with a saturated NaCl solution, anhydrified and concentrated to give 4.15 g of the title compound (yield: 97%).

1. customprepared
2. customAfter 30 minutes the solution was evaporated
3. washwashed with a cold solution of NaOH (20 ml) and water (200 ml)
4. extractionextracted in ethyl ether (twice) and ethyl acetate (once)
5. washThe organic phase was washed with a saturated NaCl solution
6. concentrationconcentrated