Ethyl chloroformate → HCID 13799984, compound

Participants

Reaction Steps

366.5 g (1.043 mol) 4-(4-Fluorobenzyl)-2-(N-methyl-piperidin-4-yl)-1-(2H)-phtalazinone are dissolved in 1100 ml toluene which had been dried over K2CO3. Any water present in azeotropically distilled off using a water separator. 390 g (3.59 mol) ethylchloroformate are added dropwise over 11/2 hours and the mixture stirred for 4 hours under reflux. A precipitate separated out and is suction filtered. The filtrate is evaporated on a rotary evaporator, the residue is taken up in 400 ml ether, stirred briefly and suction filtered. After washing with ether, the substance is dried in a drying cupboard. (M.p. 151°-152° C.).

Provenance & Evidence