Hydrochloric Acid → HCID 20453410, compound

Participants

Reaction Steps

A mixture of conc. HCl (15 ml) and water (8 ml) was added to N-methyl-8-(thiophen-2-yl)-1,4-dioxaspiro[4.5]decan-8-amine (2 g, 7.9 mmole) and stirred for 5 days at RT. The reaction mixture was worked up by dilution with water (30 ml) and extraction with ether. The ethereal phase was discarded. The aqueous phase was then made alkaline with 2N NaOH and extracted with dichloromethane (3×30 ml). The organic phase thereby obtained was dried over Na2SO4 and then concentrated by evaporation on a rotary evaporator. The residue was purified by column chromatography (silica gel 60 (50 g); 500 ml ethyl acetate/ethanol (5:1)] and Ket-4 was obtained in a yield of 1.4 g (85%) as a solid with a melting point of 72°-74° C.

Provenance & Evidence