反应详情

A solution of 1-(3,5-dichloro-pyridin-4-ylmethyl)-6-methoxy-phthalazine (1 g, 3.13 mmoles), prepared as described in example 5, in dry CH2Cl2 (15 ml), under stirring and N2 at room temperature, was added with m-chloroperbenzoic acid (0.81 g, 4.7 mmoles). After 1 hour the mixture was washed with 10% NaOH and water, anhydrified and brought to dryness. The residue was flash chromatographed (eluent: ethyl acetate 100%, then ethyl acetate/CH3OH 8:2) to give a solid which was crystallised from acetic acid/ethyl acetate to give 0.32 g of the title compound (yield: 31%). m.p.>230° C.

1. washAfter 1 hour the mixture was washed with 10% NaOH and water
2. customchromatographed (eluent
3. customethyl acetate 100%, then ethyl acetate/CH3OH 8:2) to give a solid which
4. customwas crystallised from acetic acid/ethyl acetate