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Preparation method of carbocalcitonin

A technology based on calcitonin and resin, applied in the field of synthetic peptides, can solve the problems of "three wastes" polluting the environment, low purity of crude products, and low yield, and achieve the effect of improving the purity of crude products, simple process, and high product yield

Active Publication Date: 2020-12-11
HANGZHOU GOTOP BIOTECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the traditional production process, the purity of the crude product is low and the yield is low, and even multiple separations and purifications are required to obtain qualified elcitonin
However, low yield and high cost are not conducive to large-scale production, and will produce a large amount of "three wastes" to pollute the environment

Method used

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  • Preparation method of carbocalcitonin
  • Preparation method of carbocalcitonin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Embodiment 1: A kind of preparation method of elcitonin;

[0031] Specific steps are as follows:

[0032] 1) Weigh Sieber Amide Resin (30g) with a substitution degree of 1mmol / g and put it into the reaction kettle, add an appropriate amount of DCM to swell for 20min, drain it, wash it with DMF for 3 times, and then add an appropriate amount of decapping solution (DBLK / The volume ratio of DMF is 1:4) to react for 5min and 10min in turn, and wash once with DMF in the middle. Weigh Fmoc-Pro-OH (13.65g) and TBTU (19.27g) and dissolve them thoroughly in an appropriate amount of DMF, slowly add DIEA (19.83ml) under ice-bath conditions, stir while adding, stir well and then add to the above reaction kettle , stirred and reacted at room temperature for 2 hours, then pumped dry, washed with an appropriate amount of DMF for 3 times, added 25ml of acetic anhydride / pyridine (volume ratio 1:1) to the reactor, added an appropriate amount of DMF, and then stirred and reacted at room...

Embodiment 2

[0039] Embodiment 2: A kind of preparation method of elcitonin;

[0040] Specific steps are as follows:

[0041] 1) Weigh Sieber Amide Resin (30g) with a substitution degree of 1mmol / g and put it into the reaction kettle, add an appropriate amount of DCM to swell for 20min, drain it, wash it with DMF for 3 times, and then add an appropriate amount of decapping solution (DBLK / The volume ratio of DMF is 1:4) to react for 5min and 10min in turn, and wash once with DMF in the middle. Weigh Fmoc-Pro-OH (14.17g) and TBTU (19.27g) and dissolve them thoroughly in an appropriate amount of DMF, slowly add DIEA (19.83ml) under ice bath conditions, stir while adding, and add to the above reaction kettle after stirring evenly , stirred and reacted at room temperature for 2 hours, then pumped dry, washed with an appropriate amount of DMF for 3 times, added 25ml of acetic anhydride / pyridine (volume ratio 1:1) to the reactor, added an appropriate amount of DMF, and then stirred and reacted ...

Embodiment 3

[0049] A kind of preparation method of elcitonin

[0050] Specific steps are as follows:

[0051] 1) Weigh Sieber Amide Resin (30g) with a substitution degree of 1mmol / g and put it into the reaction kettle, add an appropriate amount of DCM to swell for 20min, drain it, wash it with DMF for 3 times, and then add an appropriate amount of decapping solution (DBLK / The volume ratio of DMF is 1:4) to react for 5min and 10min in turn, and wash once with DMF in the middle. Weigh Fmoc-Pro-OH (13.15g) and TBTU (19.27g) and dissolve them thoroughly in an appropriate amount of DMF, slowly add DIEA (19.83ml) under ice bath conditions, stir while adding, stir well and then add to the above reaction kettle , stirred and reacted at room temperature for 2 hours, then pumped dry, washed with an appropriate amount of DMF for 3 times, added 25ml of acetic anhydride / pyridine (volume ratio 1:1) to the reactor, added an appropriate amount of DMF, and then stirred and reacted at room temperature fo...

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Abstract

The invention provides a preparation method of carbocalcitonin. The preparation method comprises the following steps of: (1), enabling Fmoc-Pro-OH to react with Sieber Amide Resin; (2), sequentially coupling to the last amino acid Fmoc-Ser(tBu)-OH on Fmoc-Pro-Sieber Amide Resin according to a carbocalcitonin sequence; (3), removing a side chain protecting group OAll on amino acid Asu of peptide resin, removing Fmoc to obtain a linear carbocalcitonin resin peptide with the side chain protecting group, and enabling the linear carbocalcitonin with the protecting group to fall off from the resin;(4), adjusting the solution to be neutral, removing DCM, and adding Cl-HOBT to fully react with DIC; (5), adding water to separate out the cyclic carbocalcitonin with the side chain protecting group,adding lysis solution, and adding ice ether to precipitate; and (6), preparing, separating and purifying to obtain liquid carbocalcitonin with qualified purity, converting the solution into salt to form acetate, and freeze-drying to obtain refined carbocalcitonin. The preparation method disclosed by the invention is simple; cyclization reaction is carried out under a liquid phase condition; therefore, the purity of a crude product is greatly improved; the yield of the carbocalcitonin is effectively improved; and the cost and the emission of the three wastes are reduced.

Description

technical field [0001] The invention relates to a method for synthesizing polypeptides, in particular to a method for preparing elcitonin. Background technique [0002] Calcitonin (Carbocalcitonin) is a derivative of synthetic eel calcitonin. In clinical research, the drug with Calcitonin as the main raw material can prevent bone calcium loss and improve bone quality. loose effect. [0003] Calcitonin is a polypeptide consisting of 31 amino acids, which contains a fragment with a ring structure, and the amino group on the first amino acid Ser at the N-terminus is combined with the side chain carboxyl group of the sixth amino acid Asu at the N-terminus to form an amide bond. , thus forming a relatively stable ring structure. The sequence of ercalcitonin is as follows: [0004] [Ser-Asn-Leu-Ser-Thr-Asu]-Val-Leu-Gly-Lys-Leu-Ser-Gln-Glu-Leu-His-Lys-Leu-Gln-Thr-Tyr-Pro-Arg-Thr- Asp-Val-Gly-Ala-Gly-Thr-Pro-OH, (Ser-AsuLacton); Cas. No.: 60731-46-6, molecular formula: C148H244N...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07K14/585C07K1/04C07K1/06
CPCC07K14/585Y02P20/55
Inventor 沈永刚肖攀谢振亮程益明沈永良王克霜
Owner HANGZHOU GOTOP BIOTECH
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