Hydrogen Bromide → HCID 20162901, compound

Participants

Reaction Steps

6 grams (0.013 mole) of 4-(4-chlorobenzyl)-2-(hexahydroazepin-4-yl)-1-(2H)-phthalazinone× HBr were stirred together with 3.6 grams (0.026 mole) of K2CO3, 7.4 grams (0.078 mole=7.1 ml) of 2-chloroethyl methyl ether and 30 ml of dimethylacetamide for 21/2 hours at an oil bath temperature of 120° C. Subsequently the mixture was cooled to room temperature and filtered off with suction from the insolubles. The solution was concentrated in a vacuum and the brownish oil obtained chromatographed by means of a silica gel column (elution agent: CH2Cl2 /CH3OH=90:10). The desired fractions were combined and the solvent distilled off on the rotary evaporator. The oily residue was made acid with isopropanol/HCl. The hydrochloride was precipitated as a viscous mass by addition of ether. After decanting off the supernatant solution the residue was triburated with methyl ethyl ketone at boiling heat, whereby the desired hydrochloride was obtained as a crystalline product. M.P. 194°-197° C. Yield: 1.8 grams (28%).

Provenance & Evidence