反应详情

2.00 equivalents water and 1 equivalent Arg (Mw=174.2) were mixed with DMF and stirred at room temperature until a solution was obtained. 1.03 equivalents of Z-Trp-OSu (Mw=435.45; purity=98%) were dissolved in DMF and poured in the arginine solution. Stirring was then continued at room temperature for at least 5 hours. After checking the termination of the reaction by HPLC, the reaction mixture was precipitated by adding slowly cold acetonitrile (0±5° C.) and kept at this temperature for at least 30 minutes before filtration. The precipitate was washed 3 times with a mixture of CH3CN/IPE(Isopropylether) (1/1) and then 2 times with IPE. The solid was then dried in vacuo at 45° C. A white solid was finally obtained.

1. customwas obtained
2. stirringStirring
3. waitwas then continued at room temperature for at least 5 hours
4. customthe termination of the reaction by HPLC
5. customthe reaction mixture was precipitated
6. additionby adding slowly cold acetonitrile (0±5° C.)
7. filtrationkept at this temperature for at least 30 minutes before filtration
8. washThe precipitate was washed 3 times
9. additionwith a mixture of CH3CN/IPE(Isopropylether) (1/1)
10. customThe solid was then dried in vacuo at 45° C
11. customA white solid was finally obtained