1-Methylpiperazine → HCID 18381682, compound

Participants

Reaction Steps

A solution of 4-chloro-1-(3,5-dichloro-pyridin-4-ylmethyl)-6-methoxy-phthalazine (1 g, 2.82 mmoles), prepared as described in example 45, in DMF (25 ml) was stirred under dry N2 at room temperature, and dropwise added with 1-methylpiperazine (0.848 g, 8.46 mmoles). The mixture was heated at 100° C. for 20 hours, then brought to small volume and partitioned between water and CH2Cl2. The organic phase was washed with water, anhydrified and concentrated to give a residue which was flash chromatographed (eluent: CH2Cl2/CH3OH/NH4OH 95:5:0.5). The resultant solid was crystallised from tert-butyl-methyl ether (35 ml) to give 0.4 g of the title compound (yield: 34%). m.p.: 160-162° C.

Provenance & Evidence