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Method for preparing triptorelin acetate through specific microwave synthesis

A technology of triptorelin acetate and microwave synthesis, which is applied in the field of synthesis and preparation of polypeptide drugs, can solve the problems of only triptorelin total yield, unfavorable large-scale production, complicated purification methods, etc., and achieve simplified process flow and efficient Good for mass production and high product yield

Inactive Publication Date: 2017-02-15
合肥国肽生物科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] Disadvantages: multiple cuts are required in the synthesis process, the synthesis cycle is long, and the process is complicated
[0009] Disadvantage: the total yield of triptorelin obtained is only about 25%
[0011] Disadvantages: the purification method is complicated, the purification time is long, the production cost is high, and it is not conducive to large-scale production;
[0013] Disadvantage: the total yield of triptorelin is only about 30%

Method used

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  • Method for preparing triptorelin acetate through specific microwave synthesis
  • Method for preparing triptorelin acetate through specific microwave synthesis
  • Method for preparing triptorelin acetate through specific microwave synthesis

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Embodiment 1

[0035] Embodiment 1: the method that specific microwave synthesis prepares triptorelin acetate, operation steps are as follows:

[0036] (1): Preparation of the target amino resin of the starting resin carrier

[0037] Add 0.1 g of Rink Amide-AM Resin amino resin with a substitution degree of 0.38mmol / g into the polypeptide synthesis reactor from the open end, take the DCM reagent and add it to the reactor, so that the resin is completely immersed in the DCM solvent, and the solvent Full contact, swelling for 2 hours;

[0038] After the amino resin solution is drained, add 1 / 3 of the reactor volume of 20% piperidine and DMF mixed solution, place on a 30r / min decolorizing shaker and shake for 20min, then use a vacuum pump to drain the deprotection solution; Add 1 / 3 of the DMF solution of the reactor volume, place it on a decolorizing shaker and shake for 1 min, drain the solution with a vacuum pump, add DMF solution again to wash the resin, and repeat the operation twice; use ...

Embodiment 2

[0058] (1): Preparation of the target amino resin of the starting resin carrier

[0059] Add 2 g of Rink Amide-AM Resin amino resin with a degree of substitution of 0.45 mmol / g into the polypeptide synthesis reactor from the open end, take the DCM reagent and add it to the reactor, so that the resin is completely immersed in the DCM solvent, fully mixed with the solvent Contact, swelling for 8h;

[0060] After the amino resin solution is drained, add 1 / 2 of the reactor volume of 20% piperidine and DMF mixed solution, place on a 30r / min decolorizing shaker and shake for 20min, then use a vacuum pump to drain the deprotection solution; Add DMF solution of 1 / 2 the volume of the reactor, place it on a decolorizing shaker and shake for 90s, drain the solution with a vacuum pump, add DMF solution again to wash the resin, repeat the operation twice, use ninhydrin for color detection, and obtain target amino resin;

[0061] (2): Preparation of protected amino acids

[0062] Put the...

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Abstract

The invention discloses a method for preparing triptorelin acetate through specific microwave synthesis. The method includes the following operation steps that firstly, Rink Amide-AM Resin amino resin which is obtained after swelling, deprotection and washing and has the substitution degree of 0.3-0.5 mmol / g serves as an initiative resin carrier and sequentially reacts with an activated protected amino acid solution in a constant-temperature oscillator to obtain triptorelin precursor peptide I-amino resin; secondly, a triptorelin precursor peptide I-amino resin solution is deprotected and washed to obtain solid particles, the solid particles are used for a cutting reaction, and a triptorelin crude peptide II is obtained through sediment; thirdly, the triptorelin crude peptide II is purified, a C4 filler preparation column is used, the A phase, which is 0.1% acetic acid / water and the B phase, namely 0.1% acetic acid / acetonitrile serve as a mobile phase, separation and extraction of polypeptides are conducted according to the elution gradient process of B.Cone / %:5-70,0-60 min, and pure polypeptides are obtained. The purification technology is used, product purity reaches 99%, the yield is 50% or above, the production period is shortened, and mass production is facilitated.

Description

technical field [0001] The invention belongs to the technical field of synthesis and preparation methods of polypeptide drugs, and in particular relates to a method for preparing triptorelin acetate through specific microwave synthesis. Background technique [0002] Chinese name: Triptorelin acetate, English name: Triptorelin Acetate [0003] Structural formula: Pyr-His-Trp-Ser-Tyr-D-Trp-Leu-Arg-Pro-Gly-NH2 HAC Molecular formula: C 64 h 82 N 18 o 13 , molecular weight: 1311.46. [0004] Triptorelin acetate is a synthetic analogue of luteinizing hormone releasing hormone. On the basis of natural LHRH, D-Trp is used to replace the Gly on the sixth position of the LHRH peptide chain to produce a biological activity. Strong synthetic gonadotropin-releasing hormone analogue, whose structure has been modified to enhance its affinity for pituitary receptors and slow down the inactivation of target tissues, and has a longer half-life in vivo compared to native LHRH and greater...

Claims

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Application Information

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IPC IPC(8): C07K7/23C07K1/20C07K1/06C07K1/04
CPCC07K7/23
Inventor 张旭光陈为光孙良玉郑范娜汤磊
Owner 合肥国肽生物科技有限公司
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