A kind of method for preparing peregrine
A liquid-phase and solid-phase synthesis technology, applied in the preparation methods of peptides, chemical instruments and methods, animal/human peptides, etc., can solve the problems of unsuitability for large-scale production, low purity and yield, and long synthesis cycle. and other problems, to achieve the effect of low cost, low cost and short synthesis cycle
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Embodiment 1
[0064] Example 1: Synthesis of Fmoc-Lys(Boc)-OSu Activated Ester
[0065] Weigh 468.50g Fmoc-Lys(Boc)-OH (1.0mol), add 138.10g HOSu (1.2mol) into 2000ml DMF, add 247.59g DCC (1.2mol) under ice-water bath, react for 1 hour, heat up to room temperature for 3 hours , the reaction solution was filtered, the mother liquor was spin-dried, dissolved in DCM, filtered, recrystallized from ice ethanol three times, filtered, and the solid oil pump was dried to obtain 503.37g of Fmoc-Lys(Boc)-OSu activated ester with a yield of 89%.
Embodiment 2
[0066] Example 2: Synthesis of Fmoc-Lys(Boc)-Lys(Boc)-OH
[0067] Weigh 123.15g H-Lys(Boc)-OH (0.5mol), 282.79g Fmoc-Lys(Boc)-OSu (0.5mol) and 79.50g Na 2 CO 3 (0.75mol) was added to a mixed solution of 500ml water and 500ml THF to dissolve, react overnight at room temperature, adjust the pH to 7 with 10% dilute hydrochloric acid, remove THF by rotary evaporation, and then adjust the pH to 3. A large white precipitate was obtained which was filtered. The obtained white precipitate is recrystallized with glacial ethanol, and the obtained solid oil pump is dried to obtain 296.15g of Fmoc-Lys(Boc)-Lys(Boc)-OH and its HPLC spectrogram is as follows: figure 2 Shown, HPLC purity is 98.95%, yield 85%; Its mass spectrum is as image 3 Shown, [M+Na] + : 719.525, [M+K] + : 735.773, the theoretical exact molecular weight of the dipeptide fragment Fmoc-Lys(Boc)-Lys(Boc)-OH is: 696.37, the mass spectrometry result of the sample is consistent with the theoretical molecular weight, and...
Embodiment 3
[0068] Embodiment three: adopting degree of substitution is the synthesis of the Rink Amide AM resin of 0.10mmol / g to Fmoc-Lys(Boc)-Lys(Boc)-Rink Amide AM resin
[0069] Weigh 100.00 g of Rink amide AM resin (10 mmol) with a substitution degree of 0.10 mmol / g, add it to a solid-phase reaction column, wash it once with DMF, and swell the resin with DCM for 30 minutes, and use a volume ratio of 1:4 The deprotection solution composed of piperidine and DMF was reacted for 5 minutes, washed once with DMF, reacted for 10 minutes with the deprotection solution composed of piperidine and DMF with a volume ratio of 1:4, washed 6 times with DMF, and weighed 20.91g Fmoc -Lys(Boc)-Lys(Boc)-OH (30mmol) and 4.05g HOBt (30mmol) were added to the mixed solution of DCM and DMF with a volume ratio of 1:1, and 3.79g DIC (30mmol) was added under ice-water bath for activation and then added to the above In the reaction column that resin is housed, react for 2 hours, wash 3 times with DMF, DCM wash...
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