反应详情

Methanesulfonyl chloride (0.56 g, 4.7 mmol) was added to a stirred solution of tert-butyl trans-4-aminocyclohexylcarbamate (J. Org. Chem. 8811, 61, 1996) (1.0 g, 4.7 mmol) and N-ethyl-N-isopropyl-2-propanamine (0.67 g, 0.52 mmol) in dichloromethane (30 ml). The reaction mixture was stirred for 30 min at room temperature and then partitioned between ethyl acetate (300 ml) and water (100 ml). The organic layer was washed twice with 1 molar aqueous citric acid solution and then with a saturated aqueous solution of sodium hydrogen carbonate, dried with anhydrous sodium sulfate and the solvent removed under reduced pressure to give a residue that was triturated with diethyl ether to give the title compound (0.99 g) as a white solid.

1. custompartitioned between ethyl acetate (300 ml) and water (100 ml)
2. washThe organic layer was washed twice with 1 molar aqueous citric acid solution
3. dry with materialwith a saturated aqueous solution of sodium hydrogen carbonate, dried with anhydrous sodium sulfate
4. customthe solvent removed under reduced pressure
5. customto give a residue that
6. customwas triturated with diethyl ether