反应详情

To a solution of 205 mg (0.932 mmol) of Phe(3-tBu)-NH2, 351 mg (1.21 mmol) of Boc-Cha-OH, 164 mg (1.21 mmol) of HOBT and 148 mg (1.21 mmol) of DMAP in 4 ml of DMF, 232 mg (1.21 mmol) of WSCI.HCl was added under cooling with ice and the mixture was stirred at room temperature for 1 hour. The reaction mixture was diluted with ethyl acetate and washed first with saturated aqueous NaHCO3, then with water and finally with saturated brine. The organic layer was dried with anhydrous magnesium sulfate and concentrated under reduced pressure; the resulting residue was subjected to silica gel column chromatography (eluting solvent; ethyl acetate:n-hexane=2:1) to give Boc-Cha-Phe(3-tBu)-NH2 in the amount of 326 mg (74%).

1. temperatureunder cooling with ice
2. washwashed first with saturated aqueous NaHCO3
3. dry with materialThe organic layer was dried with anhydrous magnesium sulfate
4. concentrationconcentrated under reduced pressure
5. washthe resulting residue was subjected to silica gel column chromatography (eluting solvent; ethyl acetate:n-hexane=2:1)