Potassium Iodide → HCID 21973233, compound

Participants

Reaction Steps

2.72 g (12.9 millimoles) of 5-(2-chloroethylamino)-2H-pyridazine-3-one-hydrochloride, 11 ml of anhydrous dimethyl formamide, 5.0 g (22.7 millimoles) of 6-fluoro-3-piperidine-4-yl-1,2-benzisoxazole, 6.3 ml of triethyl amine and 0.21 g of potassium iodide are admixed. The reaction mixture is heated to boiling under stirring for 8 hours, cooled to room temperature and filtered. To the mother lye a solution of 2.6 g of sodium hydrogen carbonate and 40 ml of water is added dropwise. The precipitate is filtered, suspended in 100 ml of dichloro methane, stirred for 30 minutes and filtered. The crude product is recrystallized from a 4:1 mixture of water and acetonitrile. The crystals are filtered off. Thus 2.98 g of the desired compound are obtained. Yield 64.6%. M.p.: 97–99° C.

Provenance & Evidence