反应详情

To 1-cyclopropylmethyl-4-[2-(3,3,5,5-tetramethylcyclohexyl)phenyl]piperazine (304 mg, 0.857 mmol) were added methyl alcohol (2.5 mL) and p-toluenesulfonic acid monohydrate (166 mg, 0.874 mmol) to form a thoroughly dissolved sate, and the mixture was concentrated under reduced pressure. To the obtained residual oil was added ethyl acetate to form a thoroughly dissolved state, and the mixture was allowed to stand at room temperature overnight. The suspension containing precipitated crystals was concentrated to dryness under 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 447 mg of the title compound as colorless crystals.

1. customto form a thoroughly dissolved sate
2. concentrationthe mixture was concentrated under reduced pressure
3. additionTo the obtained residual oil was added ethyl acetate
4. customto form a thoroughly dissolved state
5. additionThe suspension containing
6. customprecipitated crystals
7. concentrationwas concentrated to dryness under reduced pressure
8. additionDiethyl ether was added
9. customthe solid was triturated by sonication
10. customPrecipitated crystals
11. filtrationwere collected by filtration
12. washwashed with diethyl ether
13. customDrying under reduced pressure
14. customat room temperature