反应详情

8.1 g (20 mmol) of phenylmethyl 1-aminocyclohexanecarboxylate ·p-toluenesulfonate was added to 50 nm of water, and then 4.1 g (20 mmol) of 4-methoxybenzenesulfonylchloride and 50 ml of ethyl acetate was added to the mixture with stirring. After stirring at room temperature, the reaction mixture was put into a separatory funnel and water layer was removed therefrom. Subsequently, organic layer was washed with successive, 10% potassium hydrogensulfate solution, and saturated brine, and then, was dried over anhydrous magnesium sulfate, and the solvent was concentrated under reduced pressure. The obtained crystal was stirred overnight in ether, whereby 4.36 g of phenylmethyl 1-[N-(4-methoxybenzenesulfonyl)amino]cyclohexanecarboxylate was obtained.

1. stirringAfter stirring at room temperature
2. customthe reaction mixture was put into a separatory funnel
3. customwater layer was removed
4. washSubsequently, organic layer was washed with successive, 10% potassium hydrogensulfate solution, and saturated brine
5. dry with materialwas dried over anhydrous magnesium sulfate
6. concentrationthe solvent was concentrated under reduced pressure
7. stirringThe obtained crystal was stirred overnight in ether