Oligopeptide having marrow hemopoiesis protection function, preparation thereof, pharmaceutical composition containing the oligopeptide and use
A technology of bone marrow hematopoiesis and composition, which is applied in the field of medicine, can solve the problems of poor feasibility of large-scale production, high synthesis investment, and difficulty in developing into practical drugs, and achieve the effect of poor purity and ideal purity
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Embodiment 1
[0066] The synthesis of embodiment 1 Ac-Ser-Asp-Lys-Pro-NHEt (1)
[0067] ①Synthesis of Boc-Pro-acetophenone (Pac)-resin
[0068] Weigh 10g (5mmol) Pac-resin (substitution equivalent 0.5mmol / g, particle size 100-200 mesh, crosslinking degree 1%), three times (15mmol) moles of Boc-Pro-OH, three times the moles of K 2 CO 3 and 1 / 10 mole (0.5 mmol) of KI were mixed together with 150 mL of DMF in a round bottom flask. Under the conditions of heating and rotating in an air bath at 70°C, the reaction was carried out for 24 hours. The reaction suspension was transferred to a filter with a suction filter sand plate, and washed 5 times with DMF at 60° C., about 50 mL each time. This was followed by diafiltration with the following solvents (× times): 95% EtOH × 3, DMF × 3, 50% EtOH / H 2 O×3, anhydrous EtOH×3, anhydrous Et 2 O×2. After the solvent was drained, the resin was taken out and air-dried to constant weight under infrared light at about 50°C. Weighed Boc-Pro-OCH 2 - 10.6...
Embodiment 2
[0084] Example 2 (2) Synthesis
[0085] ① Synthesis of Fmoc-Lys(Boc)-Pac-resin
[0086] Since the Fmoc group cannot tolerate K 2 CO 3 / 60°C, in this example, DIEA equivalent to Fmoc-Lys(Boc)-OH was used instead of K 2 CO 3 , the temperature was changed to room temperature, the reaction time was extended to 35h, and all the other operations were identical to the conditions of (1) in Example 1. As a result, 11.57 g of Fmoc-Lys(Boc)-Pac-resin was obtained, with a weight gain of 1.57 g (theoretical amount: 1.938 g), and an actual yield of 81%.
[0087] ②Synthesis of Ac-Ser(tBu)-Asp(tBu)-Lys(Boc)-Pac-resin
[0088] Take 2g of Fmoc-Lys(Boc)-Pac-resin, and obtain 2.25g of Acated fully protected resin according to the conditions of Example 1 (3)-(6).
[0089] ③ piperidine aminolysis to remove the resin, preparation of
[0090] The above fully protected tripeptide resin was mixed with 8mL piperidine and 8mL THF in a sealable reaction tube and rotated on an air bath at 50°C f...
Embodiment 3
[0093] Example 3 Synthesis of Ac-Ser-Asp-Lys-NHEt (3)
[0094] The synthesis method and conditions are the same as in Example 1. Finally, 311 mg of product 3 (theoretical amount: 410 mg) was obtained, with a total yield of 75.8%, and the structure confirmed by FAB-MS: 418.4 (M+H).
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