反应详情

A solution of 4-(3,5-dichloro-pyridin-4-ylmethyl)-7-methoxy-1,2-dihydro-phthalazine (0.4 g, 1.24 mmoles), prepared as described in example 22, in glacial acetic acid (8 ml), under stirring and dry N2 at room temperature, was added with potassium cyanate (0.2 g, 2.48 mmoles) and the reaction mixture was left to stand for 20 hours, then poured into 10% NaOH in excess and extracted more times with CH2Cl2. The organic phases were washed with water, anhydrified and concentrated to give a residue which was flash chromatographed (eluent: hexane/ethyl acetate 3:7) to give 0.36 g of the title compound (yield: 80%). m.p.>230° C.

1. waitthe reaction mixture was left
2. extractionextracted more times with CH2Cl2
3. washThe organic phases were washed with water, anhydrified
4. concentrationconcentrated
5. customto give a residue which
6. customchromatographed (eluent: hexane/ethyl acetate 3:7)