反应详情

To a solution of Z-Phe-OH (742 mg) in THF (3 ml), isobutyl chloroformate (0.32 ml) and NMM (0.27 ml) were added under cooling with ice and the mixture was stirred for 15 minutes. Subsequently, a solution of N-Me-Val-N-Me-Tyr(3-tBu)-NH2 (600 mg) in THF (3 ml) was added and the mixture was stirred at room temperature for 10 hours. Water was added to the reaction mixture and extraction was effected with ethyl acetate. The extract was washed with saturated brine, dried with sodium sulfate, and concentrated under reduced pressure. The resulting residue was subjected to silica gel column chromatography (eluting solvent; n-hexane:acetone=3:2) to give Z-Phe-N-Me-Val-N-Me-Tyr(3-tBu)-NH2 in the amount of 611 mg (58%).

1. temperatureunder cooling with ice
2. stirringthe mixture was stirred at room temperature for 10 hours
3. washThe extract was washed with saturated brine
4. dry with materialdried with sodium sulfate
5. concentrationconcentrated under reduced pressure
6. washThe resulting residue was subjected to silica gel column chromatography (eluting solvent; n-hexane:acetone=3:2)