反应详情

温度

25 °C

Two solutions were prepared before the peptide coupling. Solution A: H-Gly-OH (1.2 eq.) was dissolved in MSA (3.0 eq.) at maximum 60° C. The suspension was cooled down to 25° C., diluted with DCM and stirred for at least 8 hours before being cooled to −15° C. In solution B, the carboxylic function of the Z-Glp-Pro-OH was dissolved with DCM and NMM (1.05 eq.). The solution was cooled to −15° C. The carboxylic acid was activated with IBCF (1.05 eq.) and the silylated solution A was then added to the slurry. The slurry was stirred for at least 0.5 h and left to warm to 25° C. The mixture was quenched with water and the addition of a solution of KHSO4 under stirring precipitated the peptide. The solid was filtered and washed with water. After drying under vacuum, 80% of Z-Glp-Pro-Gly-OH was recovered.

1. temperaturebefore being cooled to −15° C
2. temperatureThe solution was cooled to −15° C
3. stirringThe slurry was stirred for at least 0.5 h
4. waitleft
5. temperatureto warm to 25° C
6. customThe mixture was quenched with water
7. additionthe addition of a solution of KHSO4
8. stirringunder stirring
9. customprecipitated the peptide
10. filtrationThe solid was filtered
11. washwashed with water
12. dry with materialAfter drying under vacuum, 80% of Z-Glp-Pro-Gly-OH
13. customwas recovered