反应详情

80 mg of Z-Phe-His-Leu-Val-Ile-His-Lys(BOC)-OMe (Example 55) are dissolved in 800 μl of 95% trifluoroacetic acid (duration approximately 1 minute) and left to stand for 2 minutes. The product is then precipitated by the addition of 8 ml of diisopropyl ether, left to stand for 15 minutes at 0°, filtered off, and the precipitate is washed with diisopropyl ether and dried over KOH in a high vacuum. The powder is then dissolved in 1 ml of 90trifluoroethanol, precipitated by the addition of 10 ml of 3% MaHCO3 solution, filtered off, washed with H2O and dried over potassium hydroxide and phosphorus pentoxide in a high vacuum. To convert the resulting acid-free title compound into the acetate, the product is dissolved in 2 ml of 90% acetic acid and lyophilised. The title compound is a chromatographically homogeneous amorphous powder; Rf (B17)=0.08, Rf (B21)=0.65.

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2. customThe product is then precipitated by the addition of 8 ml of diisopropyl ether
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4. waitto stand for 15 minutes at 0°
5. filtrationfiltered off
6. washthe precipitate is washed with diisopropyl ether
7. dry with materialdried over KOH in a high vacuum
8. dissolutionThe powder is then dissolved in 1 ml of 90trifluoroethanol
9. customprecipitated by the addition of 10 ml of 3% MaHCO3 solution
10. filtrationfiltered off
11. washwashed with H2O
12. dry with materialdried over potassium hydroxide and phosphorus pentoxide in a high vacuum
13. dissolutionthe product is dissolved in 2 ml of 90% acetic acid