Preparation method of acid-sensitive ion channel inhibitor
A technology of ion channels and inhibitors, applied in the field of biological agents, can solve the problems of limited number and types of analogues, achieve the effects of shortening the synthesis cycle, improving synthesis efficiency, and complete coupling reactions
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Embodiment 1
[0077] Peptide Resin H-[36-42]-Wang resin with Protecting Group on Side Chain
[0078] 1. Fmoc-Asp (O t Synthesis of Bu)-Wang resin
[0079] (1) Wang resin (Xi'an Lanxiao Science and Technology New Materials Co., Ltd., substitution degree 1.0-1.1mmol / g, 20g) was put into the solid-phase reaction column, washed twice with DMF, and swelled in DMF for 30 minutes.
[0080] (2) Fmoc-Asp(O t Bu)-OH (9.20g, 22.35mmol), HOBt (3.02g, 22.35) were dissolved in DMF (30mL), DCM (30mL), added DIPCDI (7.52ml, 47.99mmol), pre-reacted in ice bath for 10 minutes.
[0081] (3) Add the above reaction solution into a solid-phase reaction kettle, stir it mechanically, and react at room temperature for 3 hrs. The ninhydrin detection shows that the resin is colorless and transparent.
[0082] (4) drain the solution, the resin is washed three times with DMF, DCM is washed three times, methanol shrinks three times, and vacuum is fully exhausted to obtain Fmoc-Asp(O t Bu)-Wang resin, the measured subs...
Embodiment 2
[0093] Peptide resin Fmoc-[11-21]-CTC resin with protective groups on the side chain
[0094] 1. Synthesis of Fmoc-Gly-CTC resin
[0095] Weigh 10 g of CTC resin with a substitution degree of 1.1 mmol / g, add it to a solid-phase reactor, and wash it twice with DMF. Weigh 4.45g (15mmol) of Fmoc-Gly-OH, add 120mL of DMF to dissolve, then add 9.9mL (60mmol) of DIPEA, stir for 5min, add to the solid phase reactor, and react for 2 hours. The reaction solution was drained and washed three times with DMF. Add a mixture of 20 mL methanol, 60 mL DMF and 5 mL DIPEA, and block for 30 min. Wash 3 times with DMF, twice with DCM, twice with methanol, and drain. 12.3 g of Fmoc-Gly-CTC resin was obtained, and the degree of substitution was measured to be 0.75 mmol / g.
[0096] 2. Synthesis of Fmoc-[26-35]-CTC resin
[0097] (1) Put 20g of Fmoc-Gly-CTC resin into a solid phase reactor, wash with DMF three times, and swell with DMF for 20 minutes.
[0098] (2) Drain the solution, add 2% (g / ...
Embodiment 3
[0106] Cut Fmoc-[26-35]-OH from Fmoc-[26-35]-CTC Resin:
[0107] Add 200 mL of 1% TFA in DCM to 30 g of Fmoc-[26-35]-CTC resin, and stir for 2 hours. After the reaction, filter the resin, collect the filtrate, add 20% DIPEA / DCM solution to neutralize until the pH value is about 7. The DCM was spun off, the precipitate was washed with water and ether, centrifuged and dried to give 12 g of Fmoc-[26-35]-OH.
[0108] Repeat the above operations to obtain Fmoc-[12-25]-OH and Boc-[1-11]-OH.
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