反应详情

To 1-cyclopropylmethyl-4-[2-(3,3,5,5-tetramethylcyclohexyl)phenyl]piperazine (300 mg, 0.846 mmol) were added ethyl alcohol (2.5 mL), 97% sulfuric acid (85.5 mg, 0.846 mmol) and ethyl acetate to form a thoroughly dissolved sate, and the mixture was slowly concentrated to dryness while adjusting reduced pressure. Diethyl ether was added thereto, 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 368 mg of the title compound as colorless crystals (crystal a).

1. customto form a thoroughly dissolved sate
2. concentrationthe mixture was slowly concentrated to dryness
3. additionDiethyl ether was added
4. customthe solid was triturated by sonication
5. customPrecipitated crystals
6. filtrationwere collected by filtration
7. washwashed with diethyl ether
8. customDrying under reduced pressure
9. customat room temperature