反应详情

To a solution of Boc-His(Tos)-D-Trp(CHO)-Phe-OBzl (1.16 g) in DMF (35 ml) was added pyridinium chloride (1.6 g) at room temperature. After stirring for one and half an hour, additional pyridinium chloride (0.4 g) was added and the mixture was stirred for additional 50 minutes. After evaporation, the residue was solidified with water, filtered, washed with 2% hydrochloric acid, water, 2% sodium hydrogencarbonate, water, and dried. The powder was subjected to column chromatography on silica gel (100 g) and eluted with a mixture of chloroform and methanol (20:1). The fractions containing the object compound were combined and evaporated. The residue was dissolved in ethanol and reprecipitated with water, filtered and dried to give Boc-His-D-Trp(CHO)-Phe-OBzl (0.70 g).

1. additionwas added
2. customAfter evaporation
3. filtrationfiltered
4. washwashed with 2% hydrochloric acid, water, 2% sodium hydrogencarbonate, water
5. customdried
6. washeluted with a mixture of chloroform and methanol (20:1)
7. additionThe fractions containing the object compound
8. customevaporated
9. dissolutionThe residue was dissolved in ethanol
10. customreprecipitated with water
11. filtrationfiltered
12. customdried