反应详情

Boc-Thr-OH (1.23 g), HCl.H-D-Trp(CHO)-Phe-NMeBzl (3.0 g) and HOBT (0.757 g) were dissolved in DMF (40 ml). To this solution was added WSC (887 mg) under ice cooling and the mixture was stirred for 1.5 hours at the same temperature and overnight at room temperature. After evaporation and extraction with ethyl acetate, the organic layer was washed successively with water, diluted sodium hydrogencarbonate solution, water, 0.5N hydrochloric acid, and sodium chloride solution and dried over magnesium sulfate. The evaporated residue was crystallized from a mixed solvent of ethyl acetate and diisopropyl ether (1:1) (10 ml) with seeding and the crystals were washed out by addition of diisopropyl ether (30 ml) and dried to give Boc-Thr-D-Trp(CHO)-Phe-NMeBzl (3.64 g).

1. customAfter evaporation and extraction with ethyl acetate
2. washthe organic layer was washed successively with water, diluted sodium hydrogencarbonate solution, water, 0.5N hydrochloric acid, and sodium chloride solution
3. dry with materialdried over magnesium sulfate
4. customThe evaporated residue was crystallized from a mixed solvent of ethyl acetate and diisopropyl ether (1:1) (10 ml) with seeding
5. washthe crystals were washed out by addition of diisopropyl ether (30 ml)
6. customdried