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Method for separating terbutaline enantiomers in extracted mode through hydrophobicity phase transferring chirality

A terbutaline, hydrophobic technology, applied in the directions of organic chemistry methods, chemical instruments and methods, preparation of organic compounds, etc., can solve the problems of poor solubility, excess enantiomeric content and low yield, etc., and achieves easy operation. , The effect of stable product quality and simple process

Inactive Publication Date: 2016-02-17
HUNAN INSTITUTE OF SCIENCE AND TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] An object of the present invention is to solve the problems of poor solubility of terbutaline in the organic phase and low enantiomeric excess and yield of terbutaline enantiomers separated by single-stage chiral extraction, and proposes a method for separating terbutaline Method for Enantiomers of Terbutaline - Method for Separation of Enantiomers of Terbutaline Using Hydrophobic Phase Transfer Chiral Extraction

Method used

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  • Method for separating terbutaline enantiomers in extracted mode through hydrophobicity phase transferring chirality
  • Method for separating terbutaline enantiomers in extracted mode through hydrophobicity phase transferring chirality

Examples

Experimental program
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Effect test

Embodiment 1

[0023] Take 0.5625g (0.0025mol) terbutaline enantiomer and dissolve it in 0.1mol / L Na 2 HPO 4 / NaH 2 PO 4 Adjust the pH to 7.0 in the buffer solution (0.1mol / L of hydroxypropyl-β-cyclodextrin), and prepare a 0.5L solution with a concentration of 0.005mol / L as the feed liquid;

[0024] Dissolve 441.3g (0.3mol) hydroxypropyl-β-cyclodextrin in 0.1mol / L Na 2 HPO 4 / NaH 2 PO 4 Adjust the pH to 7.0 in the buffer solution to prepare a 3L solution with a concentration of 0.1mol / L as the water phase;

[0025] Dissolve 20.52g (0.06mol) of sodium tetraphenylborate in an organic solvent (dichloromethane, 1,2-dichloroethane, n-hexane, n-heptane, cyclohexane, n-octanol, n-heptanol). 3L organic solvent with a concentration of 0.02mol / L as the organic phase;

[0026] Connect 10-stage centrifugal extractors in series. Use a constant flow pump to first pump the heavy phase into the centrifugal extractor. When there is a solution flowing out of the heavy phase outlet, pump the light phase from the corr...

Embodiment 2

[0028] Take 0.5625g (0.0025mol) terbutaline enantiomer and dissolve it in 0.1mol / L Na 2 HPO 4 / NaH 2 PO 4 Adjust the pH (5.0, 6.0, 7.0, 8.0, 9.0) in the buffer solution (0.1mol / L for hydroxypropyl-β-cyclodextrin), and prepare a 0.5L solution with a concentration of 0.005mol / L as the feed solution phase;

[0029] Dissolve 441.3g (0.3mol) hydroxypropyl-β-cyclodextrin in 0.1mol / L Na 2 HPO 4 / NaH 2 PO 4 Adjust the pH (5.0, 6.0, 7.0, 8.0, 9.0) in the buffer solution to prepare a 3L solution with a concentration of 0.1mol / L as the water phase;

[0030] Take 20.52g (0.06mol) of sodium tetraphenylborate dissolved in n-octanol to form a 3L organic solvent with a concentration of 0.02mol / L as the organic phase;

[0031] Connect 10-stage centrifugal extractors in series. Use a constant flow pump to first pump the heavy phase into the centrifugal extractor. When there is a solution flowing out of the heavy phase outlet, pump the light phase from the corresponding inlet into the centrifugal extra...

Embodiment 3

[0033] Dissolve 0.5625g (0.0025mol) terbutaline enantiomer in 0.1mol / L Na 2 HPO 4 / NaH 2 PO 4 Adjust the pH to 7.0 in the buffer solution (0.1mol / L of hydroxypropyl-β-cyclodextrin), and prepare a 0.5L solution with a concentration of 0.005mol / L as the feed liquid;

[0034] Dissolve 441.3g (0.3mol) hydroxypropyl-β-cyclodextrin in 0.1mol / L Na 2 HPO 4 / NaH 2 PO 4 Adjust the pH to 7.0 in the buffer solution to prepare a 3L solution with a concentration of 0.1mol / L as the water phase;

[0035] Dissolve the phase transfer agent (sodium tetraphenylborate, potassium tetraphenylborate, sodium hexafluorophosphate, potassium hexafluorophosphate) in n-octanol to prepare a 3L organic solvent with a concentration of 0.02mol / L as the organic phase;

[0036] Connect a 10-stage centrifugal extractor in series, use a constant flow pump to first pump the heavy phase into the centrifugal extractor. When the heavy phase exits the solution, pump the light phase into the centrifugal extractor from the corre...

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Abstract

The invention provides a method for separating terbutaline enantiomers in an extracted mode through hydrophobicity phase transferring chirality. Beta-cyclodextrin is used as an extraction agent, the terbutaline enantiomers serve as separated objects, the solubilizing performance of a hydrophobicity phase transferring agent for terbutaline in the organic phase is used, mass transferring efficiency is improved through the centrifugal acting force of a centrifugal extractor, mass transferring and reacting of the terbutaline enantiomers in the water phase and the organic phase are accelerated, extract-phase outlet purity and raffinate-phase outlet purity are greatly improved accordingly, and the extract-phase yield and the raffinate-phase yield are greatly increased accordingly. The method has the advantages that the extraction agent and the phase transferring agent are low in price and easy to get; extraction efficiency is high, and the separating speed is high; operation is flexible, and the environment-friendly effect and the efficient effect are achieved. By means of the method, the problem that the solubility of the terbutaline in the organic phase is poor is solved, and the problems that as for common extraction technologies, mass transferring efficiency is low, single-stage extraction is carried out, and purity and the yield are low are solved. Rapid and high-selectivity separation of the terbutaline can be achieved through multi-stage counter-current extraction.

Description

Technical field [0001] The invention relates to a method for the separation of terbutaline enantiomers by hydrophobic phase transfer chiral extraction, which specifically includes using a phase transfer agent to enhance the extraction process, and then extracting and separating terbutaline pairs through a centrifugal extractor through a multi-stage countercurrent reaction. Enantiomer method. Background technique [0002] Terbutaline (Terbutaline), as β 2 Adrenergic receptor agonist, for β 2 The receptor has sympathomimetic activity. This product is a kind of bronchodilator. Its relaxing effect on the bronchus is similar to that of salbutamol, but the effect of stimulating the heart is significantly less than that of salbutamol. It can be used clinically to treat bronchial asthma, chronic bronchitis, emphysema and other lung diseases accompanied by bronchospasm. It also has a relaxing effect on uterine smooth muscle. Terbutaline is a racemic drug with a pair of enantiomers. I...

Claims

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Application Information

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IPC IPC(8): C07C213/10C07C215/30
CPCC07C213/10C07B2200/07C07C215/30
Inventor 唐课文张盼良冯晓峰许卫凤熊碧权刘宇杨长安周从山
Owner HUNAN INSTITUTE OF SCIENCE AND TECHNOLOGY
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