Phosphorus oxychloride → 4-Chloro-1-[(3,5-dichloropyridin-4-yl)methyl]-6-methoxyphthalazine

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Reaction Steps

POCl3 (22.2 ml, 230 mmoles) was added to a suspension of 4-(3,5-dichloro-pyridin-4-ylmethyl)-7-methoxy-2H-phthalazin-1-one (10 g, 25.5 mmoles), obtained as described in example 12, in acetonitrile (300 ml) and the mixture was heated under reflux. After 3 hours the solution was concentrated, taken up with CH2Cl2, with water, and the pH was brought to 7-8 with Na2CO3. The organic phases were decoloured with charcoal, dried and concentrated to give 10 g of the title compound (stoichiometric yield).

Provenance & Evidence