反应详情

1.32 g of Z-Ile-OSu [G. W. Anderson et. al., J. Amer. Chem. Soc. 86, 1839 (1964)] are dissolved in the above solution of H-His-Lys(Boc)-OMe in approximately 10 ml of DMF and mixed with 0.41 ml of NEt3. The whole is left to stand for 8 hours at room temperature, 15 ml of diisopropyl ether are added, and the whole is homogenised and filtered. The residue obtained by filtering with suction is dissolved in 15 ml of methanol and added at 0° to 23 ml of aqueous NaHCO3 solution. The resulting precipitate is filtered off, washed with H2O, dried and dissolved and reprecipitated from MeOH/ethyl acetate/petroleum ether, yielding Z-Ile-His-Lys(Boc)-OMe in the form of amorphous powder; Rf (B)=0.65; Rf (I)=0.48.

1. waitThe whole is left
2. filtrationfiltered
3. customThe residue obtained
4. filtrationby filtering with suction
5. dissolutionis dissolved in 15 ml of methanol
6. additionadded at 0° to 23 ml of aqueous NaHCO3 solution
7. filtrationThe resulting precipitate is filtered off
8. washwashed with H2O
9. customdried
10. dissolutiondissolved
11. customreprecipitated from MeOH/ethyl acetate/petroleum ether