Potassium Hydroxide → HCID 21153172, compound

Participants

Reaction Steps

A solution of 7.1 g of the product of Step A in 70 ml of n-butanol was mixed with stirring under nitrogen with 7 g of potassium hydroxide pastilles and the mixture was then refluxed for 17 hours. The mixture was evaporated to dryness and the residue was taken up in methylene chloride. The solution was washed with water and dried and evaporated to dryness to obtain 5.5 g of cis N-methyl-5-[4-trifluoromethylphenoxy]-6,7,8,9-tetrahydro-5H-benzocyclohepten-7-amine in the form of an orange oil. The latter was dissolved in 30 ml of ethyl acetate and the solution was made acidic by addition of a solution of gaseous hydrogen chloride in ethyl acetate. Crystallized was effected and the mixture was vacuum filtered. The recovered product was washed with ethyl acetate and was dried to obtain 5.4 g of the hydrochloride of the cis product in the form of white crystals melting at ≈220° C.

Provenance & Evidence