反应详情

温度

12.5 °C

To a solution of biotinamido-N-methylglycyl-serine t-butyl ester (6) in anhydrous dimethylformamide is added 3 equivalents of triethylamine, 0.01-0.1 equivalents of 4-dimethylaminopyridine and 1.1 equivalents of succinic anhydride. The mixture is stirred at 0-25° C. for 20-24 h and then concentrated via reduced pressure rotary evaporation. The residue is diluted with ethyl acetate and 1 N aqueous hydrochloric acid. The organic phase is then dried over magnesium sulfate, filtered and concentrated. The residue is chromatographed on reverse phase C-18 silica gel, eluting with methanol/water. The fractions containing the product are combined and concentrated to give the final product (4).

1. concentrationconcentrated via reduced pressure rotary evaporation
2. additionThe residue is diluted with ethyl acetate and 1 N aqueous hydrochloric acid
3. dry with materialThe organic phase is then dried over magnesium sulfate
4. filtrationfiltered
5. concentrationconcentrated
6. customThe residue is chromatographed on reverse phase C-18 silica gel
7. washeluting with methanol/water
8. additionThe fractions containing the product
9. concentrationconcentrated