反应详情

温度

0 °C

To a cold (0° C.) solution of Boc-D-Phe-OH (5 g) in N,N-dimethyl formamide (200 ml) were successively added 1-hydroxy benzotriazole (4.29 g), dicyclohexyl carbodimide (4.29 g), H-Pro-OMe.HCl (3.1 g) and N-ethylmorpholine (3 ml). The mixture was stirred at 0° C. for 1 hour and then kept at room temperature for 2 days. The mixture was cooled to −20° C. and dicyclohexylurea was removed by filtration. The filtrate was evaporated to dryness. The residue was dissolved in ethyl acetate and washed successively with 5% sodium hydrogen carbonate, 0.1M hydrogen chloride-solution, saturated aqueous sodium chloride, dried over sodium sulfate and concentrated in vacuo. The residue was chromatographed on silica gel in heptane/ethyl acetate=6/4 (v/v) as eluent. The fractions containing Boc-D-Phe-Pro-OMe were pooled and evaporated. Yield: 1.5 g.

1. waitkept at room temperature for 2 days
2. temperatureThe mixture was cooled to −20° C.
3. customdicyclohexylurea was removed by filtration
4. customThe filtrate was evaporated to dryness
5. dissolutionThe residue was dissolved in ethyl acetate
6. washwashed successively with 5% sodium hydrogen carbonate, 0.1M hydrogen chloride-solution, saturated aqueous sodium chloride
7. dry with materialdried over sodium sulfate
8. concentrationconcentrated in vacuo
9. customThe residue was chromatographed on silica gel in heptane/ethyl acetate=6/4 (v/v) as eluent
10. additionThe fractions containing Boc-D-Phe-Pro-OMe
11. customevaporated