Chloroform → HCID 21285201, compound

Participants

Reaction Steps

A mixture of 24.77 g (0.0676 M) of 1-(3-chlorophenyl)-3-(hydroxymethyl)-6,7-dimethoxy-isoquinoline hydrochloride (compound of Example 1), 150 ml of chloroform and 10.1 g (13.9 ml, 0.1 M) of triethylamine is refluxed for 15 minutes. After cooling the solution is extracted with 3×50 ml of water, the chloroform layer is dried over anhydrous sodium sulfate, evaporated, giving the aimed product in crystalline, base form. This base is purified by dissolving in 25 ml of hot 99.5% ethanol. After cooling the resulting crystalline mass is mixed with 25 ml of diethyl ether, cooled, filtered, washed with 3×5 ml of a mixture (1:1) of ethanol and ether, and subsequently dried at 60° to 80° C. Yield 16.73 g (75.1%), m.p. 118° to 120° C.

Provenance & Evidence