Dimethylformamide → HCID 18504799, compound

Participants

Reaction Steps

A solution under nitrogen of 3,5-dichloro-4-methyl-pyridine (457 mg, 2.82 mmoles) in dry DMF (10 ml) was portionwise added with 60% NaH (113 mg, 2.82 mmoles) and, after 1 hour at room temperature, was dropwise added, at a temperature <10° C., with 1-chloro-6-difluoromethoxy-5-(tetrahydrofuran-2-yloxy)-phthalazine (296 mg, 0.937 mmoles), obtained as described in example 53, in dry DMF (10 ml). After 2 hours at room temperature the mixture was poured into a 0.4M buffer at pH=7 (50 ml), extracted in ethyl acetate (2×50 ml) and the organic phase was washed with water, anhydrified and concentrated under vacuum. The residue was chromatographed (eluent:benzene/ethyl acetate 1:1, then ethyl acetate only), then crystallized from ethyl ether/benzene to give 180 mg of the title product (yield: 43.5%).

Provenance & Evidence