反应详情

To a solution of 4-(t-butoxycarbonylamino)-1-(4-piperidinylmethyl)piperidine (590 mg) in methylene chloride (30 ml) is added trimethylsilyl isocyanate (220 mg) under ice-cooling, and the mixture is stirred at room temperature for 8 hours. The reaction mixture is washed with water and a saturated aqueous sodium chloride solution, dried over anhydrous magnesium sulfate, and the solvent is evaporated under reduced pressure. The residue is purified by silica gel column chromatography (eluent; chloroform:methanol=10:1) to give 4-(t-butoxycarbonylamino)-1-(1-carbamoyl-4-piperidinylmethyl)piperidine (540 mg).

1. temperaturecooling
2. washThe reaction mixture is washed with water
3. dry with materiala saturated aqueous sodium chloride solution, dried over anhydrous magnesium sulfate
4. customthe solvent is evaporated under reduced pressure
5. customThe residue is purified by silica gel column chromatography (eluent; chloroform:methanol=10:1)