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Alpha-cyano benzalcohol and alpha-cyano benzalcohol acetate mixture extraction and separation method

A technology of cyanobenzyl alcohol acetate and cyanobenzyl alcohol, which is applied in the field of extraction and separation of mixtures of α-cyanobenzyl alcohol and α-cyanobenzyl alcohol acetate, to achieve the effect of easy source, low price, and stability

Inactive Publication Date: 2007-08-15
ZHEJIANG UNIV
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  • Summary
  • Abstract
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  • Application Information

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Problems solved by technology

The main ways to obtain α-cyanobenzyl alcohol are asymmetric synthesis and racemate resolution. Early research mainly focused on chemical synthesis and resolution. In recent years, biological preparation methods have gradually received attention, especially the application of organic phase enzyme catalysis. To make the enzymatic synthesis and resolution of α-cyanobenzyl alcohol more practical, the commonly used organic phase enzyme-catalyzed methods include lipase-catalyzed selective esterification resolution and lipase-catalyzed asymmetric alcoholysis resolution. A method, in order to obtain high-purity α-cyanobenzyl alcohol, the separation of α-cyanobenzyl alcohol and α-cyanobenzyl alcohol acetate must be carried out, and there is no bibliographical information for this content at present

Method used

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  • Alpha-cyano benzalcohol and alpha-cyano benzalcohol acetate mixture extraction and separation method

Examples

Experimental program
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Effect test

Embodiment 1

[0012] The extractant is n-hexane and hydrochloric acid solution with pH=2, methanol is a co-solvent, the volume percentage of each component is 50%, 49% and 1% respectively, and the total volume is 2L. Add 32g of benzyl alcohol and racemic α-cyanobenzyl alcohol acetate to the extractant at 30°C, shake fully, let stand for 30rin, separate the upper and lower phases, and carry out secondary and tertiary extractions under the same conditions , the upper phase is dehydrated with anhydrous sodium sulfate and distilled under reduced pressure at 40°C to obtain α-cyanobenzyl alcohol acetate with a recovery rate of 85.73% and a purity of 95.48%; the lower phase is distilled under reduced pressure at 40°C When the volume remains constant, back-extract with an equal volume of ether, take the upper phase of the back-extraction, dehydrate with anhydrous sodium sulfate, and distill under reduced pressure at 40°C to obtain α-cyanobenzyl alcohol with a recovery rate of 89.12% and a purity of ...

Embodiment 2

[0014] The extractant is n-hexane and sulfuric acid solution with pH=1, ethanol is used as co-solvent, the volume percentage of each component is 50%, 40% and 10% respectively, the total volume is 400mL, and the racemic α-cyano group is added in equimolar ratio The mixture of benzyl alcohol acetate and racemic α-cyanobenzyl alcohol is 9.4g. After three stages of continuous extraction at 40°C, the upper phase is dehydrated with anhydrous sodium sulfate and distilled under reduced pressure at 50°C to obtain α-cyanobenzyl alcohol. Benzyl alcohol acetate, the recovery rate is 83.05%, and the purity is 92.37%; the lower phase is distilled under reduced pressure at 50°C until the volume remains constant, back extracted with an equal volume of ether, the upper phase of the back extraction is taken, and dehydrated with anhydrous sodium sulfate , Distilled under reduced pressure at 50°C to obtain α-cyanobenzyl alcohol with a recovery rate of 82.52% and a purity of 89.45%.

Embodiment 3

[0016] Extractant is the citric acid solution of normal hexane and pH=2, and methanol is cosolvent, and each component volume percent is respectively 50%, 45% and 5%, and total volume is 500mL, and adding molar ratio is 3: 1 (S 10.8g of the mixture of )-α-cyanobenzyl alcohol and (R)-α-cyanobenzyl alcohol acetate, after three stages of continuous extraction at 20°C, was processed according to the method of Example 1 to obtain (R) The recovery rate of -α-cyanobenzyl alcohol acetate was 83.89%, and the purity was 94.56%; the recovery rate of (S)-α-cyanobenzyl alcohol was 83.70%, and the purity was 90.12%.

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Abstract

The invention discloses the extraction separation method for the mixture of alpha-cyano benzylalcohol and alpha-cyano benzylalcohol acetate. The method comprises the following steps: .using the methanol or ethanol as assisting solvent, direct adding the racemic or optics pure mixture of alpha-cyano benzylalcohol and alpha-cyano benzylalcohol acetate into the extracting agent which is composed of skellysolve B, and acid water solution (pH<=3), vibrating, intimate mixing, carrying out single-stage or multi-speed extracting, stewing, layering, separating the two phases; after dehydrating the above phase by anhydrous sodium sulfate, vacuum distilling ,and getting the alpha-cyano benzylalcohol acetate; vacuum distilling under phase, extracting the under phase with ether as reextracting agent, after dehydrating the strip liquor, vacuum distilling, and getting the alpha-cyano benzylalcohol. In the invention, the technology is simple, the cost of manufacture is low, the price of extractant is cheap, and the economic benefit is good.

Description

technical field [0001] The invention relates to a method for extracting and separating alpha-cyanobenzyl alcohol and alpha-cyanobenzyl alcohol acetate mixture. Background technique [0002] α-cyanobenzyl alcohol is an extremely important fine chemical intermediate, which can generate dozens of important fine chemicals such as amine compounds, hydroxyl compounds, carboxyl compounds, etc., and is called a universal chiral intermediate. According to reports, there is a potential market of 3,000-4,000 tons of α-cyanobenzyl alcohol series derivatives in the world, and most of them are high-value-added, high-tech products with considerable development potential, which have attracted much attention. The main ways to obtain α-cyanobenzyl alcohol are asymmetric synthesis and racemate resolution. Early research mainly focused on chemical synthesis and resolution. In recent years, biological preparation methods have gradually received attention, especially the application of organic ph...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C255/53C07C253/34
Inventor 杨立荣熊健徐刚吴坚平
Owner ZHEJIANG UNIV
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