反应详情

To a solution of the thus obtained Tyr(3-tBu)-NH2 (1 g, 4.23 mmol), Z-N-Me-Val-OH (1.23 g, 4.63 mmol) and CMPI (1.2 g, 4.69 mmol) in THF (20 ml), TEA (1.8 ml) was added under cooling with ice and stirred at room temperature for 4 hours. The reaction mixture was mixed with water and extracted with ethyl acetate. The organic layer was washed with saturated brine, dried over sodium sulfate and evaporated to remove the solvent under reduced pressure; the thus obtained residue was subjected to silica gel column chromatography (developing solvent: ethyl acetate:n-hexane=2:1), giving Z-N-Me-Val-Tyr(3-tBu)-NH2 (1.7 g, 83%).

1. temperatureunder cooling with ice
2. extractionextracted with ethyl acetate
3. washThe organic layer was washed with saturated brine
4. dry with materialdried over sodium sulfate
5. customevaporated
6. customto remove the solvent under reduced pressure