反应详情

To 1-cyclopropylmethyl-4-[2-(3,3,5,5-tetramethylcyclohexyl)phenyl]piperazine (306 mg, 0.863 mmol) were added methyl alcohol (3 mL) and 47% hydrobromic acid (152 mg, 0.888 mmol) to form a thoroughly dissolved sate. Ethyl acetate was slowly added thereto at room temperature to precipitate crystals, then the suspension was concentrated to dryness under reduced pressure. A mixed solvent of diethyl ether and ethyl acetate 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 375 mg of the title compound as colorless crystals.

1. customto form a thoroughly dissolved sate
2. customat room temperature to precipitate crystals
3. concentrationthe suspension was concentrated to dryness under reduced pressure
4. additionA mixed solvent of diethyl ether and ethyl acetate was added
5. customthe solid was triturated by sonication
6. customPrecipitated crystals
7. filtrationwere collected by filtration
8. washwashed with diethyl ether
9. customDrying under reduced pressure
10. customat room temperature