反应详情

2.3 g (8.64 mmole) quantity of N,N'-dicyclohexylcarbodiimide was added to 20 ml of a solution of 2.0 g (7.35 mmole) of N-decylpiperazine hydrochloride, 1.9 g (7.56 mmole) of N-t-butoxycarbonylphenylglycine, 1.3 g (15.5 mmole) of sodium hydrogencarbonate and 122 mg (1.0 mmole) of 4-dimethylaminopyridine in anhydrous methylene chloride. The mixture was stirred at room temperature for 12 hours. The precipitated crystals were collected by filtration and washed with methylene chloride. Mother liquor and the washings were combined and concentrated under reduced pressure and the residue was purified by silica gel chromatography (chloroform : methanol =15 : 1), giving 2.8 g (yield: 83 %) of 1-(N-t-butoxycarbonyl-phenylglycyl)-4-decylpiperazine.

1. filtrationThe precipitated crystals were collected by filtration
2. washwashed with methylene chloride
3. concentrationconcentrated under reduced pressure
4. customthe residue was purified by silica gel chromatography (chloroform : methanol =15 : 1)