Peptides containing tyr-val fragments, their synthesis, activity and application
A technology of -obzl-asp-tyr-val-obzl, heptapeptide is applied to peptides containing Tyr-Val fragments, and its synthesis, activity and application fields can solve problems such as not being obtained
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Embodiment 1
[0062] Embodiment 1 prepares Boc-Tyr-Val-OBzl
[0063] Under ice bath, 2.81g (10mmol) Boc-Tyr was dissolved in a small amount of anhydrous tetrahydrofuran (THF), 1.36g (10mmol) HOBt was added, and a solution of 2.47g (12mmol) DCC and a small amount of anhydrous THF was added, and activated for 30 minutes. Add 2.07g (10mmol) Val-OBzl, use NMM to adjust pH=9, and filter to remove dicyclohexyl urea (DCU) after the reaction is completed. The filtrate was concentrated under reduced pressure, the residue was dissolved in ethyl acetate, the DCU was filtered again, and the filtrate was dissolved in NaHCO 3 Wash 3 times with saturated solution, wash 3 times with saturated NaCl solution, 5% KHSO 4 solution washed 3 times, NaCl saturated solution washed 3 times, 5% NaHCO 3 The solution was extracted and washed 3 times, the NaCl saturated solution was extracted and washed 3 times, and the ethyl acetate layer was washed with anhydrous NaCl 2 SO 4 Dry for 12 hours, filter off Na 2 SO ...
Embodiment 2
[0064] Embodiment 2 prepares Tyr-Val-OBzl
[0065] Dissolve 4.7g (10mmol) Boc-Tyr-Val-OBzl with a small amount of dried ethyl acetate under ice bath, stir for 10min, add 50mL hydrogen chloride-ethyl acetate solution (4N) to react for 4h, and the raw material point disappears. The reaction mixture was concentrated to dryness under reduced pressure, and the residue was dissolved in 40 mL of dried ethyl acetate, and the resulting solution was concentrated to dryness under reduced pressure. This operation was repeated 3 times for the residue. Add anhydrous diethyl ether to the residue, grind with a plastic spatula, and concentrate under reduced pressure to remove diethyl ether. This operation was repeated 3 times for the residue. Obtained 3.97 g (99%) of the title compound as a colorless powder. ESI + -MS (m / e): 372 [M+H] + .
Embodiment 3
[0066]Embodiment 3 prepares Boc-Leu-Phe-OBzl
[0067] According to the method of Example 1, 2.31 g (10 mmol) Boc-Leu and 2.55 g (10 mmol) Phe-OBzl gave 3.98 g (81.6%) of the title compound as a colorless oil. ESI + -MS(m / e): 470[M+H] + .
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