反应详情

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).

1. customto form a thoroughly dissolved sate
2. concentrationfollowed by concentration under reduced pressure
3. additionTo the obtained residual oil was added ethyl acetate
4. dissolutionto dissolve again
5. additionThe suspension containing
6. customprecipitated crystals
7. concentrationwas concentrated to dryness under reduced pressure
8. additionA mixed solvent of diethyl ether and ethyl acetate was added to the suspension
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