2-Chloroethyldiisopropylammonium chloride → HCID 21293328, compound

Participants

Reaction Steps

6-Bromo-2-[3-(dimethylamino)propyl]phthalazin-1(2H)-one (8.5 gm) (prepared as in Example I, except that 3-(dimethylamino)propyl chloride hydrochloride was substituted for the 2-(diisopropylamino)ethyl chloride hydrochloride) was stirred into 4 ml DMSO plus 4 ml acetonitrile. To the resulting mixture was added 3.7 gm 4-methylthiostyrene, 0.2 gm tri(O-tolyl)phosphine, and 0.04 gm palladium acetate. The reaction mixture was stirred at reflux (95°-100° C.) for 24 hours. The solution was concentrated to dryness on a rotovap and the residue recrystallized from 95% ethanol yielding 5.5 gm of product melting at 210° C.

Provenance & Evidence