Ethanol → HCID 11719403, compound

Participants

Reaction Steps

To 1-cyclopropylmethyl-4-[2-(3,3,5,5-tetramethylcyclohexyl)phenyl]piperazine (310 mg, 0.874 mmol) were added ethyl alcohol (2.5 mL), 97% sulfuric acid (44.2 mg, 0.437 mmol) and ethyl acetate to form a thoroughly dissolved sate, followed by concentration under reduced pressure. To the obtained residual oil was added ethyl acetate to dissolve again, and the mixture was allowed to stand. The suspension containing precipitated crystals was concentrated to dryness under reduced pressure. A mixed solvent of diethyl ether and ethyl acetate was added to the suspension, and the solid was triturated by sonication. Precipitated crystals were collected by filtration, washed with diethyl ether, and aircured by aspiration. Drying under reduced pressure using a vacuum pump at room temperature gave 209 mg of the title compound as colorless crystals (crystal b).

Provenance & Evidence