反应详情

温度

5 °C

DMA, 1.05 equivalents of DIPEA (Mw=129.2) and 1.05 equivalents of H-Trp-Pro-OH (Mw=301.3; purity=91.0%) were mixed at room temperature for at least 30 min until a solution had formed. The reaction mixture was then diluted with ethyl acetate and cooled to 5±5° C. Once this temperature was reached, 1.00 equivalent of Z-Trp-OSu (Mw=435.45; purity=98.0%) was added and stirring continued for at least 30 min before the solution was left to warm up to room temperature again. After the completion of the reaction was confirmed by HPLC, 0.2 eq of, DMAPA (N,N′-Dimethylaminopropylamine, Mw=102.2 g/mol) were added. The reaction mixture was diluted with ethyl acetate and washed with a 5% (weight) aqueous NaCl solution containing 2 equivalents of KHSO4. The organic phase was further washed first with a 5% (weight) aqueous NaCl solution and finally with water. The organic phase was partially concentrated in vacuo and the residue was suspended in ethyl acetate and further concentrated in order to eliminate the remaining water. The concentrated peptide solution was added in small portions to a cold (0±5° C.) mixture of MTBE/petroleum ether (45-55) (1/1) and the precipitate was kept at 0±5° C. for at least 30 min before filtration. After filtration, it was then washed with petroleum ether (45-55) and dried in vacuo at 45° C. A white solid was finally obtained.

1. customhad formed
2. waitcontinued for at least 30 min before the solution
3. waitwas left
4. temperatureto warm up to room temperature again
5. additionwere added
6. washwashed with a 5% (weight) aqueous NaCl solution
7. washThe organic phase was further washed first with a 5% (weight) aqueous NaCl solution and finally with water
8. concentrationThe organic phase was partially concentrated in vacuo
9. concentrationfurther concentrated in order
10. additionThe concentrated peptide solution was added in small portions to a cold (0±5° C.) mixture of MTBE/petroleum ether (45-55) (1/1)
11. filtrationthe precipitate was kept at 0±5° C. for at least 30 min before filtration
12. filtrationAfter filtration, it
13. washwas then washed with petroleum ether (45-55)
14. customdried in vacuo at 45° C
15. customA white solid was finally obtained