Method for separating and purifying temsirolimus

A technology for separation and purification of temsirolimus, applied in the field of separation and purification of generic drugs, can solve the problems of inflammable and explosive, unsuitable for industrialized large-scale production, low boiling point of diethyl ether, etc. Effect

Active Publication Date: 2019-06-07
YANGTZE RIVER PHARM GRP SICHUAN HAIRONG PHARM CO LTD
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Problems solved by technology

[0003] It can be seen from the reported literature that there are few studies on the separation and purification of temsirolimus at present. The isomer content can be reduced to less than 1.0% by recrystallization, but ether has a low boiling point and is flammable and explosive, so it is not suitable for use. in industrialized mass production

Method used

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  • Method for separating and purifying temsirolimus
  • Method for separating and purifying temsirolimus
  • Method for separating and purifying temsirolimus

Examples

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Embodiment 1

[0026] Embodiment 1 Separation and purification of temsirolimus of the present invention

[0027] a. Dissolve 2,2,5-trimethyl-5-carboxylic acid-1,3-dioxane in n-hexane, add thionyl chloride at 25±5°C, mix the mass volume ratio m 2,2,5-三甲基-5-羧酸-1,3-二氧六烷 :V 正己烷 :m 二氯亚砜 =1g: 14ml: 1.37g, stirred for 15h. Concentrate to dryness under reduced pressure to obtain a colorless oily liquid, the acid chloride.

[0028] b. Mix rapamycin, N, N-diisopropylethylamine (DIPEA) with dichloromethane (DCM), its mass volume ratio m 雷帕霉素 :V DIPEA :V DCM =1g: 0.72ml: 2.83ml, drop the acid chloride prepared in the above a at 0-5°C, so that the concentration of the acid chloride is 1g / ml, stir and react at 25±5°C for 22h, then take a sample, and detect the content of rapamycin by HPLC After less than 0.5%, concentrated and evaporated to dryness, the obtained crude product was purified by 200-300 mesh column silica gel with petroleum ether: ethyl acetate 1:1 as eluent, and the esterified product ...

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Abstract

The invention discloses a method for separating and purifying temsirolimus. The method comprises the following steps: (1) synthesis of a crude product; and (2) separation and purification. The specific separation and purification method has the advantages of great improvement of the purity and the yield of temsirolimus, reduction of the cost, and broad market application prospect.

Description

technical field [0001] The invention belongs to the field of separation and purification of generic drugs, in particular to a method for separation and purification of temsirolimus. Background technique [0002] Temsirolimus (Temsirolimus) (Temsirolimus) (Temsirolimus) (Temsirolimus) (Temsirolimus) is an intravenous injection of mTOR inhibitors, approved for the treatment of advanced renal cell carcinoma, is a derivative and prodrug of sirolimus. Tesirolimus uses rapamycin (sirolimus) as a raw material, through esterification, deprotection and other synthetic processes to generate temsirolimus finished product with low purity and high isomer content. Most of the current research reports are the separation and purification methods of rapamycin (sirolimus) (CN104844620A, CN107619413A, etc.). According to reaxys search, there are few reports on the isolation and purification of temsirolimus. Zheng Congshen et al. announced a refinement study of temsirolimus in the "13th Natio...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D498/18
Inventor 曹康平孙建谢义鹏刘艳霞
Owner YANGTZE RIVER PHARM GRP SICHUAN HAIRONG PHARM CO LTD
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