Supercharge Your Innovation With Domain-Expert AI Agents!

Method for separating and purifying Fmoc-Gly-Thr(psi(Me,Me)pro)-OH in large scales

A separation and purification, large-scale technology, applied in the chemical industry, can solve the problems of high product failure rate, long cycle time, and many process steps, etc., and achieve the effect of improving the pass rate, short production cycle, and high purification efficiency

Inactive Publication Date: 2019-03-26
HANGZHOU GOTOP BIOTECH
View PDF2 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] At present, the preparation method of the pseudo dipeptide Fmoc-Gly-Thr(ψ(Me,Me)pro)-OH generally adopts the synthetic method, and the synthetic method has the following disadvantages: the process has many steps, the cycle is long, and the reflux reaction in the middle is easy to cause the product The racemization of the product makes the defective rate of the product after synthesis higher, and in the synthesis process, it needs to use dangerous reagents such as flammable, explosive and high toxicity, which has high cost, poor comprehensive benefit, and serious pollution of three wastes

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] A method for large-scale separation and purification of pseudo dipeptide Fmoc-Gly-Thr (ψ(Me, Me)pro)-OH, comprising the steps of:

[0022] Step 1: Crude product treatment: Dissolve 60 g of Fmoc-Gly-Thr(ψ(Me, Me)pro)-OH crude product in 3 L of methanol aqueous solution with a volume ratio of methanol:water=4:1 and form a mixed solution , and then carry out ultrasonic treatment to the mixed solution, until the mixed solution is completely clarified, filter the mixed solution through membrane filtration, and then collect the filtrate for later use;

[0023] Step 2: Use high-performance liquid chromatography to separate and purify the filtrate obtained in step 1: select DAC-HB200 dynamic axial compression column as the chromatographic column, and process the filtrate obtained in step 1 through DAC-HB200 dynamic axial compression column Isogradient elution separates and purifies and obtains samples, and uses ultraviolet detectors to detect samples, and collects high-concentr...

Embodiment 2

[0035] A method for large-scale separation and purification of pseudo dipeptide Fmoc-Gly-Thr (ψ(Me, Me)pro)-OH, comprising the steps of:

[0036] Step 1: Crude product treatment: Dissolve 70 g of the Fmoc-Gly-Thr(ψ(Me, Me)pro)-OH crude product in 3 L of methanol aqueous solution with a volume ratio of methanol:water=4:1 and form a mixed solution , and then carry out ultrasonic treatment to the mixed solution, until the mixed solution is completely clarified, filter the mixed solution through membrane filtration, and then collect the filtrate for later use;

[0037] Step 2: Use high-performance liquid chromatography to separate and purify the filtrate obtained in step 1: select DAC-HB200 dynamic axial compression column as the chromatographic column, and process the filtrate obtained in step 1 through DAC-HB200 dynamic axial compression column Isogradient elution separates and purifies and obtains samples, and uses ultraviolet detectors to detect samples, and collects high-conc...

Embodiment 3

[0049] A method for large-scale separation and purification of pseudo dipeptide Fmoc-Gly-Thr (ψ(Me, Me)pro)-OH, comprising the steps of:

[0050] Step 1: Crude product treatment: Dissolve 80g of Fmoc-Gly-Thr(ψ(Me,Me)pro)-OH crude product in 3L methanol aqueous solution with a volume ratio of methanol:water=4:1 and form a mixed solution , and then carry out ultrasonic treatment to the mixed solution, until the mixed solution is completely clarified, filter the mixed solution through membrane filtration, and then collect the filtrate for later use;

[0051] Step 2: Use high-performance liquid chromatography to separate and purify the filtrate obtained in step 1: select DAC-HB200 dynamic axial compression column as the chromatographic column, and process the filtrate obtained in step 1 through DAC-HB200 dynamic axial compression column Isogradient elution separates and purifies and obtains samples, and uses ultraviolet detectors to detect samples, and collects high-concentration ...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

PropertyMeasurementUnit
Lengthaaaaaaaaaa
Login to View More

Abstract

The invention discloses a method for separating and purifying Fmoc-Gly-Thr(psi(Me,Me)pro)-OH in large scales. The method comprises the following steps that 1, crude product treatment; 2, a high performance liquid chromatograph instrument is used for separating and purifying filtering liquid obtained in the first step; 3, a high-concentration peptide solution with the purity being 98.0 percent or higher, obtained in the second step is subjected to pressure reduction rotary evaporation concentration; concentrated liquid is collected; the concentrated liquid is subjected to freeze drying; a whiteflocculent powder product is obtained. A reversed phase high-performance liquid chromatography is used for separating and purifying the Fmoc-Gly-Thr(psi(Me,Me)pro)-OH; through an isogradient elutionseparation process of a DAC-HB200 dynamic axial compression column, the goal of producing hundreds of g of Fmoc-Gly-Thr(psi(Me,Me)pro)-OH products with the purity being 98.0 percent or higher in one step is realized; the qualified rate of the product is greatly improved; high purification efficiency is realized; the cost is reduced. The process has the advantages of simplicity, high speed and short production period, and is suitable for large-scale industrial production, popularization and application.

Description

technical field [0001] The present invention relates to the field of chemical technology, in particular to a method for large-scale separation and purification of pseudo-dipeptide Fmoc-Gly-Thr(ψ(Me,Me)pro)-OH, specifically to a method based on reversed-phase high-performance liquid phase Chromatographic large-scale separation and purification of pseudo dipeptide Fmoc-Gly-Thr(ψ(Me,Me)pro)-OH method. Background technique [0002] At present, the preparation method of the pseudo dipeptide Fmoc-Gly-Thr(ψ(Me,Me)pro)-OH generally adopts the synthetic method, and the synthetic method has the following disadvantages: the process has many steps, the cycle is long, and the reflux reaction in the middle is easy to cause the product The racemization of the product makes the defective rate of the product after synthesis higher, and in the synthesis process, it needs to use dangerous reagents such as flammable, explosive and high toxicity, which has high cost, poor comprehensive benefit, ...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
IPC IPC(8): C07K5/062C07K1/14C07K1/16C07K1/34
CPCC07K5/06026
Inventor 程益明
Owner HANGZHOU GOTOP BIOTECH
Features
  • R&D
  • Intellectual Property
  • Life Sciences
  • Materials
  • Tech Scout
Why Patsnap Eureka
  • Unparalleled Data Quality
  • Higher Quality Content
  • 60% Fewer Hallucinations
Social media
Patsnap Eureka Blog
Learn More

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic, Popular Technical Reports.

© 2025 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap|About US| Contact US: help@patsnap.com