HRID1837748
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
In acetonitrile (4 ml) were dissolved 90 mg of 1-[(2-methoxy-3-pyridyl)methyl]-4-[2-(2-methanesulfonylaminophenyl)-2-oxoethyl]piperidine obtained in Example 65 and 0.30 ml of concentrated hydrochloric acid, followed by heating under reflux for 5 hours. The solvent was evaporated, and then the residue was dissolved in ethyl acetate and an aqueous 1N sodium hydroxide. The organic layer was separated, washed with brine, and then dried over anhydrous magnesium sulfate. The solvent was evaporated, and the crude product was recrystallized from ethanol, to give 45 mg of the title compound as colorless crystals.
WORKUP
后处理
- temperatureby heating
- temperatureunder reflux for 5 hours
- customThe solvent was evaporated
- dissolutionthe residue was dissolved in ethyl acetate
- customThe organic layer was separated
- washwashed with brine
- dry with materialdried over anhydrous magnesium sulfate
- customThe solvent was evaporated
- customthe crude product was recrystallized from ethanol