反应详情

1.21 g (12 mmol) of triethylamine was added to a solution of 2.33 g (10 mmol) of 1-aminocyclohexanecarboxylic acid phenylmethyl ester in 100 ml of tetrahydrofuran, and 1.55 g (10 mmol) of phenylacetyl chloride was added dropwise to the mixture under ice-cooling, followed by stirring of the mixture overnight. Under reduced pressure, the reaction solution was concentrated, ethyl acetate was added thereto, and the mixture was successively washed with water, a 10% aqueous potassium hydrogensulfate solution, a saturated aqueous sodium hydrogencarbonate solution and saturated brine, followed by drying with anhydrous sodium sulfate. After the solvent was distilled off under reduced pressure, the residue was purified by silica gel chromatography to obtain 3.21 g (91%) of the title compound.

1. additionwas added dropwise to the mixture under ice-
2. temperaturecooling
3. concentrationUnder reduced pressure, the reaction solution was concentrated
4. additionethyl acetate was added
5. washthe mixture was successively washed with water
6. dry with materialby drying with anhydrous sodium sulfate
7. distillationAfter the solvent was distilled off under reduced pressure
8. customthe residue was purified by silica gel chromatography