反应详情

Dicyclohexylcarbodiimide (1.58 g) was added to an ice-cooled solution of 2.0 g of N-carbobenzyloxyserine, 1.57 g of 1-(3-phenylpropyl)piperazine and 1.04 g of 1-hydroxybenzotiazole in 30 ml of N,N-dimethylformamide. The mixture was stirred at room temperature for 24 hours, then diluted with ethyl acetate, washed in sequence with two portions of 4% aqueous sodium hydrogen carbonate, one portion of water and one portion of saturated aqueous solution of sodium chloride, dried over anhydrous sodium sulfate and concentrated under reduced pressure. The residue was purified by silica gel column chromatography to give 2.39 g of 1-[2-(benzyloxycarbonylamino)-3-hydroxypropionyl]-4-(3-phenylpropyl}piperazine. Melting point 95°-97° C.

1. washwashed in sequence with two portions of 4% aqueous sodium hydrogen carbonate, one portion of water and one portion of saturated aqueous solution of sodium chloride
2. dry with materialdried over anhydrous sodium sulfate
3. concentrationconcentrated under reduced pressure
4. customThe residue was purified by silica gel column chromatography