反应详情

To a solution of 150 mg (0.642 mmol) trans-3-[4-(2-methylamino-ethyl)-cyclohexyl]-(E)-prop-2-en-1-ol HCl-salt and 125 mg (0.654 mmol) 4-chlorophenyl chloroformate in 1.5 ml of dichloromethane was added at room temperature 0.55 ml (3.21 mmol) diisopropyl ethyl amine. The reaction mixture was stirred for 1 hour at room temperature, taken up in ether and washed with 1N hydrogen chloride solution and water. The organic layer was dried over magnesium sulfate and concentrated under reduced pressure and the residue then chromatographed on silica gel with a 2:1 v/v mixture of hexane and ethylacetate as the eluent giving 146 mg (64.7%) trans-{2-[4-(3-hydroxy-(E)-propenyl)-cyclohexyl]-ethyl}-methyl-carbamic acid 4-chloro-phenyl ester, MS: 369 (MNH4+, 1Cl).

1. washwashed with 1N hydrogen chloride solution and water
2. dry with materialThe organic layer was dried over magnesium sulfate
3. concentrationconcentrated under reduced pressure
4. customthe residue then chromatographed on silica gel with a 2:1 v/v mixture of hexane and ethylacetate as the eluent