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 80 ml of chloroform were added 3.59 g of 1-methylnipecotic acid hydrochloride and 6.26 ml of triethylamine. Thereto was added 3.0 g of isobutyl chloroformate under ice cooling and stirring. The mixture was stirred for 30 minutes. Thereto was added 3.1 g of cyclooctylmethylamine, and the mixture was subjected to a reaction for 2 hours at room temperature. The reaction mixture was washed with an aqueous sodium hydrogen carbonate solution and with water, and dried with anhydrous sodium sulfate. The solvent was removed by evaporation. The residue was purified by a Silica gel column chromatography (dichloromethane:methanol=10:1) to obtain 3.3 g of 1-methyl-3-cyclooctylmethylaminocarbonylpiperidine.
WORKUP
后处理
- stirringThe mixture was stirred for 30 minutes
- customthe mixture was subjected to a reaction for 2 hours at room temperature
- washThe reaction mixture was washed with an aqueous sodium hydrogen carbonate solution and with water
- dry with materialdried with anhydrous sodium sulfate
- customThe solvent was removed by evaporation
- customThe residue was purified by a Silica gel column chromatography (dichloromethane:methanol=10:1)