Hydrochloric Acid → HCID 18381639, compound

Participants

Reaction Conditions

Reaction Steps

A suspension under N2 of [4-(3,5-dichloro-pyridin-4-ylmethyl)-6-methoxy-phthalazin-1-yl]-methanol (1.25 g, 3.6 mmoles), prepared as described in example 103, in CH2Cl2 (30 ml) was added with triethylamine (0.75 ml, 5.4 mmoles). The mixture was cooled to 0-4° C. and dropwise added with methanesulfonyl chloride (0.33 ml, 4.32 mmoles) in CH2Cl2 (5 ml). At the end of the addition the resultant solution was stirred for 1 hour at room temperature, then cooled and added with morpholine (0.94 ml, 10.8 mmoles). The mixture was stirred at room temperature for 3 hours, then poured into 5% HCl. The acidic phase was alkalinised and twice extracted with CH2Cl2, then discoloured with charcoal, filtered over celite and dried to give a foam which was flash chromatographed (eluent: CH2Cl2/CH3OH 98:2). The yielded foam was triturated in ethyl ether to give 1.1 g of the title compound (yield: 52%). m.p.: 202.6-205.6° C.

Provenance & Evidence