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Method for refining rapamycin

A technology of rapamycin and refining method, applied in the direction of organic chemistry, etc., can solve the problems of short cycle, poor product quality stability and high cost, and achieve the effect of short cycle and good product stability

Inactive Publication Date: 2019-02-22
ZHUOHE PHARM GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The purpose of the present invention is to disclose a method for refining rapamycin, which does not use a detachable column, and overcomes the problems of high cost, long cycle and poor product quality stability caused by using a detachable column in the prior art. The invention can achieve the effect of the separation column through a simple chemical method, the cycle is short, and the product stability is good

Method used

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  • Method for refining rapamycin
  • Method for refining rapamycin
  • Method for refining rapamycin

Examples

Experimental program
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Effect test

Embodiment 1

[0025] The present embodiment is to make rapamycin according to the above method, and the specific steps are as follows:

[0026] S1: 100m anhydrous dichloromethane, 9.5g rapamycin, 4g imidazole and 6.4g trimethylchlorosilane were sequentially added to a 250ml reaction bottle, stirred by magnetic force, reacted at room temperature for 12h, TLC judged that the reaction was complete, concentrated to obtain rapamycin Mycin silicone ether 11.5g.

[0027] S2: Add 10g of rapamycin silicon ether to a 250ml round-bottom flask, add 135ml of methyl tert-butyl ether / tetrahydrofuran (10 / 1), heat to reflux for 1h, heat suction filtration, and the filtrate naturally cools to room temperature and then stirs overnight at 0°C. crystal, suction filtered, and the filter cake was washed with a small amount of ethanol to obtain 8.8 g of white crystals.

[0028] S3: add 11.3 rapamycin silicon ether crystals to a 250ml reaction bottle for silica gel column chromatography, the silica gel column chro...

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Abstract

The invention provides a method for refining rapamycin. The method comprises the following steps of: S1: carrying out silyl ether protection reaction on a crude product of rapamycin with a structuralformula as shown in a formula (1) to obtain rapamycin silyl ether with a structural formula as shown in a formula (2); S2: dissolving and recrystallizing the rapamycin silyl ether obtained in the stepS1 in an alcohol solvent to obtain a rapamycin silyl ether crystal; and S3: carrying out de-protection reaction on the rapamycin silyl ether crystal obtained in the step S2 to generate a target product rapamycin with a structural formula as shown in a formula (3). The rapamycin prepared by the method for purifying rapamycin can achieve the effect of leaving a column through a simple chemical method, and is short in cycle and good in product stability.

Description

technical field [0001] The invention belongs to the technical field of pharmaceutical production, and more specifically relates to a method for refining rapamycin. Background technique [0002] Rapamycin (RAPA) is a new type of macrolide antibiotics. At first RAPA was studied as a low toxicity antifungal drug. In 1977, RAPA was found to have immunosuppressive effect. In 1989, RAPA was used as a new drug for the treatment of organ transplant rejection. RAPA blocks signal transduction through different cytokine receptors, and blocks the progress of T lymphocytes and other cells from G1 phase to S phase, thereby exerting an immunosuppressive effect. Judging from the current clinical application, RAPA has a good anti-rejection effect, and has a good synergistic effect with immunosuppressants such as cyclosporine A (CsA) and FK506. It is a drug with good curative effect, low toxicity and no nephrotoxicity. new immunosuppressant. The latest study found that RAPA is an effective...

Claims

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Application Information

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IPC IPC(8): C07D498/18
CPCC07D498/18
Inventor 王涛李晓明王庆林王彬彬孙益林
Owner ZHUOHE PHARM GRP CO LTD