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Method for synthesizing beta-ionone

A synthesis method and ionone technology, which are applied in chemical instruments and methods, preparation of organic compounds, preparation of carbon-based compounds, etc., can solve the problems of insufficient mixing of solvent and sulfuric acid, difficult control of reaction temperature, difficulty in amplification, and the like, To achieve the effect of convenient construction and operation, convenient and accurate adjustment and control, and inhibition of side reactions

Inactive Publication Date: 2008-12-31
BAYER TECH & ENG SHANGHAI
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  • Description
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Problems solved by technology

[0008] In order to solve the problems of complex operation of the current β-ionone batch reaction process, insufficient two-phase mixing of solvent and sulfuric acid, difficulty in controlling the reaction temperature, and difficulty in scaling up, the invention provides a method for continuously synthesizing β-ionone

Method used

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  • Method for synthesizing beta-ionone

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Effect test

Embodiment 1

[0030] The chloroform / pseudo-ionone volume ratio is 3 / 1 mixture 10, and the concentrated sulfuric acid 20 of 95~98wt%, with the flow rate of 15ml / h respectively, simultaneously input with pump 30 and pump 40 and place in temperature control device 50 In the microreactor 60, the reaction temperature is controlled at -2°C. The channel structure of the microreactor is a comb type, and the channel size is 75 μm. The reaction product 70 was collected with ice water, and the organic phase obtained by solvent extraction was analyzed by gas chromatography. The conversion rate of the pseudoionone cyclization reaction was 97.91wt%, and the selectivity of β-ionone was 94.96wt%.

Embodiment 2

[0032] The chloroform / pseudo-ionone volume ratio is 3 / 1 mixture 10, and the concentrated sulfuric acid 20 of 95~98wt%, with the flow rate of 30ml / min respectively, simultaneously use pump 30 and pump 40 input to be placed in temperature control device 50 In the microreactor 60, the reaction temperature is controlled at -2°C. The channel structure of the microreactor is a comb type, and the channel size is 75 μm. The reaction product 70 was collected with ice water, and the organic phase obtained by solvent extraction was analyzed by gas chromatography. The conversion rate of pseudoionone cyclization reaction was 97.87wt%, and the selectivity of β-ionone was 92.93wt%.

Embodiment 3

[0034] The chloroform / pseudo-ionone volume ratio is 6 / 1 mixture 10, and the concentrated sulfuric acid 20 of 95~98wt%, with the flow rate of 30ml / h respectively, simultaneously input with pump 30 and pump 40 and place in temperature control device 50 In the microreactor 60, the reaction temperature is controlled at -2°C. The channel structure of the microreactor is a comb type, and the channel size is 75 μm. The reaction product 70 was collected with ice water, and the organic phase obtained by solvent extraction was analyzed by gas chromatography. The conversion rate of the pseudoionone cyclization reaction was 82.41wt%, and the selectivity of β-ionone was 94.72wt%.

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Abstract

The invention relates to a method for synthesizing beta-ionone, in particular to a method which uses a micro-reactor and takes concentrated sulfuric acid as catalyst to continuously synthesize beta-ionone through cyclization reaction to pseudoionone. The synthesis method can effectively suppress side effects; the selectivity of the beta-ionone in the product is 90-97 wt%.

Description

technical field [0001] The present invention relates to the synthesis method of β-ionone. Background technique [0002] β-ionone is an important raw material for the preparation of vitamin A in the pharmaceutical industry, and can generally be synthesized by the cyclization reaction of pseudoionone under the catalysis of concentrated sulfuric acid. [0003] The traditional synthesis process of β-ionone usually adopts a batch reactor, and the pseudoionone is slowly added to the mixture of organic solvent and concentrated sulfuric acid under continuous stirring to carry out the cyclization reaction. Since the reaction occurs at the two-phase interface of the solvent phase and the sulfuric acid phase, the sufficient mixing of the two phases in the reactor can increase the reaction contact area. [0004] An increase in temperature will cause the reaction to proceed in the direction of generating α-ionone and other by-products, so the reaction temperature of the β-ionone synthes...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C49/217C07C45/67
Inventor 郭岱石付敏廖建平
Owner BAYER TECH & ENG SHANGHAI
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