Unlock instant, AI-driven research and patent intelligence for your innovation.

A kind of splitting method of pregabalin

A technology of pregabalin and lactam, applied in the field of medicinal chemistry, can solve the problems of severe reaction conditions, low yield and the like, and achieve the effects of improving purity, convenient operation, and safe and environmentally friendly separation method.

Active Publication Date: 2021-11-16
ZHUOHE PHARM GRP CO LTD
View PDF0 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The preparation of pregabalin mainly includes asymmetric synthesis and chemical resolution. Chemical resolution is the mainstream method of production today, but the yield is low and the reaction conditions are severe. The development of a mild resolution method has important application value

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

[0028] This embodiment discloses a kind of pregabalin prepared according to the above method, and the specific reaction steps are as follows:

[0029] Add 15.9g of pregabalin racemate and 300ml of acetic anhydride to a 1L reaction flask, reflux and stir for 6h, cool down to room temperature naturally, recrystallize in refrigerator, and obtain 10.7g of white solid by suction filtration. Add 15.9g of white solid and 200ml of ethyl acetate into a 05L reaction bottle, stir to dissolve, 5ml of concentrated sulfuric acid, reflux and stir for 24 hours, let it cool down to room temperature naturally, adjust the pH to 5 with 2M sodium hydroxide, concentrate, extract the residue with ethanol and put it under reflux Add cyclohexane until slightly turbid, then add ethanol dropwise until dissolved, stir and crystallize in an ice bath for 2 hours, and filter with suction to obtain 11.5 g of pregabalin lactam.

[0030] 14.1 g of pregabalin lactam was dissolved in 1.5 L of toluene, and 1 g of...

Embodiment 2

[0033] This embodiment discloses a kind of pregabalin prepared according to the above method, and the specific reaction steps are as follows:

[0034] Add 15.9g of white solid and 200ml of ethyl acetate into a 0.5L reaction bottle, stir to dissolve, 5ml of concentrated sulfuric acid, reflux and stir for 24 hours, then cool down to room temperature naturally, adjust the pH to 5 with 2M sodium hydroxide, concentrate, and extract the residue with ethanol and then reflux Add cyclohexane until slightly turbid, then add ethanol dropwise until dissolved, stir and crystallize in an ice bath for 2 hours, and filter with suction to obtain 11.5 g of pregabalin lactam.

[0035] 14.1 g of pregabalin lactam was dissolved in 1.5 L of toluene, and 1 g of lipase was added. The lipase was Novozym 435 lipase. The reaction temperature was 35° C., the reaction temperature was 24 h, and the shaker speed was 200 r / min. After suction filtration and concentration at room temperature, isopropanol was r...

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

No PUM Login to View More

Abstract

The invention provides a method for splitting pregabalin, which uses the racemate of pregabalin as a starting material to prepare a chiral ester of pregabalin under the action of lipase, and the chiral ester of pregabalin is passed through Hydrolysis reaction gives pregabalin. The pregabalin prepared by the splitting method of pregabalin in the present invention has high purity, and the splitting method is convenient to operate, and is also safer and more environmentally friendly.

Description

technical field [0001] The invention relates to the technical field of medicinal chemistry, in particular to a method for splitting pregabalin. Background technique [0002] Pregabalin is an analogue of the neurotransmitter GABA, a follow-up to gabapentin. The mechanism of action of pregabalin is similar to that of gabapentin, and it has shown anticonvulsant and analgesic effects in different animal models, but the detailed mechanism of action is still unclear. Pregabalin is structurally similar to the neurotransmitter GABA, but it does not act directly through the GABA mechanism. At the same time, this product is different from traditional antiepileptic drugs. It does not interact with GABAA or GABAB receptors within the effective concentration range. It is not metabolized into GABA or GABA agonist, nor does it inhibit the uptake and degradation of GABA, nor does it act on sodium or calcium channels, nor the release and uptake of glutamate. At the same time, pregabalin di...

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
Patent Type & Authority Patents(China)
IPC IPC(8): C07C229/08C07C227/22C07D207/267C12P13/00
CPCC07B2200/07C07C227/22C07D207/267C12P13/005C07C229/08
Inventor 王涛李晓明王庆林王彬彬孙益林
Owner ZHUOHE PHARM GRP CO LTD