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Solid phase polypeptide synthesis preparation method for salcatonin

A technology for solid-phase peptide synthesis and salmon calcitonin, which is applied to peptide preparation methods, calcitonin, chemical instruments and methods, etc., can solve the problems of complex process, high cost, and many wastes

Active Publication Date: 2006-11-22
SHANGHAI SOHO YIMING PHARMA
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  • Claims
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Problems solved by technology

[0007] U.S. Patent (USP508,382) reports a preparation method for the synthesis of salmon calcitonin by a solid-phase method: a method for synthesizing salmon calcitonin using the Bco strategy. The method disclosed in this document uses highly toxic and corrosive reagents, three wastes Many, complex process, high cost, industrial implementation has certain difficulty, can not meet the needs of clinical application

Method used

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  • Solid phase polypeptide synthesis preparation method for salcatonin

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Embodiment 1

[0257] Weigh 22 grams of Rink Amide MBHA resin (100-200 mesh, 0.85mmol / g, 18.7mmol), soak in 300ml of DMF to fully swell the resin, and blow dry with nitrogen. Add 500 ml of 20% hexahydropyridine in DMF and shake at 25°C for 30 minutes. Hexahydropyridine was blown and filtered with nitrogen, washed with DMF and three times, and dried with nitrogen.

[0258] Preparation of Fmoc-Pro-resin:

[0259] Add Fmoc-Pro-OH (MW337.4, 74.4mmol) 25.1g, TBTU (MW: 321, 74.5mmol) 23.9g, HOBT (MW: 135.1, 85.6mmol) 11.6g, NMM 16.5ml (MW = 101.2), 250ml of DMF, and the mixture was shaken at 25°C for 1 hour. Blow dry with nitrogen, wash with DMF three times, and blow dry with nitrogen.

[0260] Add 500 ml of 20% hexahydropyridine in DMF and shake at 25°C for 30 minutes. Blow dry with nitrogen, wash with DMF six times, and blow dry with nitrogen.

[0261] Preparation of Fmoc-Thr(tBu)-Pro-resin:

[0262] Add Fmoc-Thr(tBu)-OH (MW: 397.5, 74.5mmol) 29.6g, TBTU (MW: 321, 74.5mmol) 23.9g, HOBT (MW...

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Abstract

The invention discloses a new salmon calcimar preparing method of Fmoc-strategy solid-phase polypeptide, which comprises the following steps: a. adopting Fmoc-Rink Amide MBHA or Rink Amide AM resin to connect the 32-piptide resin protected by kinds of amino acid after eluting Fmoc-protection sequently; b. eluting Fmoc-protective group sequently; c. removing side-chain protective group and cutting peptide synchronously to obtain reduced crude product; d. making crude product to do oxidation reaction through (7.5-10.0 pH) air; proceeding inverse-phase HPLC separation and purifying to produce fine salmon calcimar. The invention possesses scale producing capacity, which improves the quality, obtaining rate, and total obtaining rate.

Description

technical field [0001] The invention relates to a preparation method of salmon calcitonin, in particular to a preparation method of solid-phase polypeptide synthesis of salmon calcitonin. Background technique [0002] Salmon calcitonin, English name: Calcitonin (Salmon), trade name: Miacaicic, chemical structural formula: [0003] [0004] Molecular formula and molecular weight: C 145 h 240 N 44 o 48 S 2 3431.9 [0005] Salmon calcitonin is clinically used in the treatment of osteoporosis. Natural calcitonin (CT) is a biologically active polypeptide secreted by parathyroid cells of mammals or hind parotids of non-mammalian vertebrates. It is the main regulator of calcium metabolism in organisms. It comes from humans, pigs CT extracts or synthetic products of , salmon, eel, etc. have been developed into medicines, among which salmon calcitonin (sCT) has a strong and long-lasting clinical effect, which is 32 times more active than human calcitonin (hCT) and has a lo...

Claims

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Application Information

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IPC IPC(8): C07K14/585C07K1/04
CPCY02P20/55
Inventor 周达明
Owner SHANGHAI SOHO YIMING PHARMA
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