反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
To 1-cyclopropylmethyl-4-[2-(3,3,5,5-tetramethylcyclohexyl)phenyl]piperazine (300 mg, 0.846 mmol) were added methyl alcohol (2.5 mL) and benzenesulfonic acid (136 mg, 0.863 mmol) to form a thoroughly dissolved state, followed by concentration under reduced pressure. To the obtained residual oil was added ethyl acetate to dissolve, and the mixture was allowed to stand. 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 425 mg of the title compound as colorless crystals.
WORKUP
后处理
- customto form a thoroughly dissolved state
- concentrationfollowed by concentration under reduced pressure
- additionTo the obtained residual oil was added ethyl acetate
- dissolutionto dissolve
- additionThe suspension containing
- customprecipitated crystals
- concentrationwas concentrated to dryness under reduced pressure
- additionDiethyl ether was added
- customthe solid was triturated by sonication
- customPrecipitated crystals
- filtrationwere collected by filtration
- washwashed with diethyl ether
- customDrying under reduced pressure
- customat room temperature