反应详情

To a solution of 1 (300 mg, 0.40 mmol, 1 eq) in MeCN (8 mL) was added Et2NH (0.8 mL, 10% v/v) dropwise at rt under Ar(g). The solution was stirred at rt for 2 h, then the solvent was removed in vacuo. The excess of amine was co-evaporated with MeCN (3×5 mL), then with a 1:5 mixture of CH2Cl2/hexane (10 mL). A white solid was obtained and the flask was dried under high vacuum for 2 h. To a solution of Fmoc-D-Phenylalanine (173 mg, 0.45 mmol, 1.1 eq) in MeCN (7 mL) at 0° C. was added PyBOP (233 mg, 0.45 mmol, 1.1 eq) and 176 μL of N-ethyldiisopropylamine (1.01 mmol, 2.5 eq) under Ar(g). The crude amine, dissolved in CH2Cl2 (6 mL) was added to the mixture dropwise. The reaction mixture was then left to warm to rt overnight. The mixture was then concentrated in vacuo and the residue was further purified by silica gel column chromatography with hexane/EtOAc (1:2→0:1) to yield 2 as a white solid (294 mg, 82%).

1. customthe solvent was removed in vacuo
2. additionwith a 1:5 mixture of CH2Cl2/hexane (10 mL)
3. customA white solid was obtained
4. customthe flask was dried under high vacuum for 2 h
5. additionwas added to the mixture dropwise
6. waitThe reaction mixture was then left
7. temperatureto warm to rt overnight
8. concentrationThe mixture was then concentrated in vacuo
9. customthe residue was further purified by silica gel column chromatography with hexane/EtOAc (1:2→0:1)