Water → HCID 66991117, compound

Participants

Reaction Conditions

Reaction Steps

In order to prepare the hydrochloride salt, 42 g of the base 3-[2-(dimethylamino)methyl(cyclohex-1-yl)phenol were added to 210 ml methyl ethyl ketone. Subsequently 2 ml water and 23 ml trimethylchlorosilane, dissolved in 45 ml methyl ethyl ketone, were added. The reaction mixture was cooled down to 0° C. by cooling with ice and was kept cold overnight (in a refrigerator at about 4° C.). The solid substance that precipitated out was filtered out by suction using a suction filter, with application of a vacuum, and then washed with 30 ml of acetone. The yield of 3-[2-(dimethylamino)methyl(cyclohex-1-yl)]phenol hydrochloride was 49 g (corresponding to 100% of the theoretical value). According to NMR and GC analyses, the produce was >95% trans diastereomer. The melting-point was 122-126° C.

Provenance & Evidence