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High-conversion-rate phenylacetaldehyde preparation method

A technology with high conversion rate and phenylacetaldehyde, which is applied in the preparation of heterocyclic compounds, hydrogenolysis preparation, organic chemistry, etc., can solve the problems that the output of phenylacetaldehyde cannot meet the market demand and cannot obtain high yield of phenylacetaldehyde, etc. Achieve the effect of low cost, low equipment requirements, and improved synthesis yield

Inactive Publication Date: 2017-06-13
DONGGUAN LIANZHOU INTPROP OPERATION MANAGEMENT CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the common industrial production method of phenylacetaldehyde is to prepare phenylacetaldehyde by oxidation of phenylethyl alcohol or reduction of ethyl phenylacetate. Because phenylacetaldehyde is active in nature and easy to oxidize and polymerize, the current industrial method cannot obtain high yield and high purity. Phenylacetaldehyde, with the continuous expansion of the scope of application of phenylacetaldehyde, the output of phenylacetaldehyde will be far from meeting the market demand

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] A kind of preparation method of the phenylacetaldehyde of high transformation rate, comprises the following steps:

[0028] (1) Using methyl benzoate as a raw material, the loaded zinc oxide catalyst is packed in a tubular reactor with an inner diameter of 20mm, and the catalyst is purged for 0.5h at a temperature of 400°C with hydrogen and nitrogen gas mixture. Air space velocity is 100mL / min;

[0029] After that, methyl benzoate 0.05h -1 The space-velocity liquid-phase feed, the hydrogen ester molar ratio is 1.5, and adds nitrogen, reacts at 380 ℃, 0.2MPa, makes benzaldehyde, and the transformation efficiency of methyl benzoate is 91.5%; Wherein, nitrogen and benzoic acid The molar ratio of methyl ester is 0.1:1;

[0030] (2) Benzaldehyde and ethyl chloroacetate are reacted for 50h at 15° C. under the action of alkali, tetrabutylammonium chloride and dimethylformamide to generate epoxy ester, and the productive rate of epoxy ester is 86.9%. ; Wherein, the molar rat...

Embodiment 2

[0033] A kind of preparation method of the phenylacetaldehyde of high transformation rate, comprises the following steps:

[0034] (1) Using methyl benzoate as a raw material, load the supported zinc oxide catalyst in a tubular reactor with an inner diameter of 20mm, and use hydrogen and nitrogen gas mixture to purge the catalyst for 0.7h at a temperature of 400°C. Air space velocity is 100mL / min;

[0035] After that, methyl benzoate 0.25h -1 The space velocity liquid phase feeding, the hydrogen ester molar ratio is 2, and adds nitrogen, reacts under 390 ℃, 0.3MPa, makes benzaldehyde, and the transformation rate of methyl benzoate is 91.8%; Wherein, nitrogen and benzoic acid The molar ratio of methyl ester is 3:1;

[0036] (2) Benzaldehyde and ethyl chloroacetate react 20h at 20°C under the action of alkali, trioctylmethyl ammonium chloride and dimethylacetamide to generate epoxy ester, and the productive rate of epoxy ester is 89.8%; wherein, the molar ratio of benzaldehyd...

Embodiment 3

[0039] A kind of preparation method of the phenylacetaldehyde of high transformation rate, comprises the following steps:

[0040] (1) Using methyl benzoate as a raw material, the loaded zinc oxide catalyst is packed in a tubular reactor with an inner diameter of 20mm, and the catalyst is purged for 0.5-1.5h at a temperature of 400°C with hydrogen and nitrogen gas mixture, The air velocity of the purge gas is 100mL / min;

[0041] After that, methyl benzoate 0.45h -1 The space-velocity liquid-phase feed, the hydrogen ester mol ratio is 3, and adds helium, reacts at 400 ℃, 0.4MPa, makes benzaldehyde, and the transformation efficiency of methyl benzoate is 91.7%; Wherein, helium and The molar ratio of methyl benzoate is 4:1;

[0042] (2) Benzaldehyde and ethyl chloroacetate are reacted for 30h at 25° C. under the action of alkali, dodecyltrimethylammonium chloride and tetrahydrofuran to generate epoxy ester, and the productive rate of epoxy ester is 87.9%. ; Wherein, the molar ...

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PUM

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Abstract

The invention discloses a high-conversion-rate phenylacetaldehyde preparation method. The preparation method comprises the following steps: taking methyl benzoate as a raw material, enabling the methyl benzoate to be in contact with a catalyst, performing hydrogenation reaction to generate benzaldehyde, and adding diluter into the reaction system at the same time of the reaction; reacting the benzaldehyde and ethyl chloroacetate in the presence of alkali, the catalyst and organic solvent to generate epoxy acid ester; and hydrolyzing the epoxy acid ester under an alkaline condition, and decarboxylating to obtain phenylacetaldehyde. The method has mild process conditions and low requirements for equipment; and the product is easy to separate and high in synthesis ratio.

Description

[0001] Technical field: [0002] The invention relates to the field of organic synthesis, in particular to a method for preparing phenylacetaldehyde with a high conversion rate. [0003] Background technique: [0004] Phenylacetaldehyde, an oily colorless liquid with strong hosta aroma, is a widely used intermediate in organic synthesis. In terms of spices, acetal spices can be prepared, which is an important spice blending agent; in terms of environment, Schiff base can be prepared to purify waste water; in terms of pesticides, it is an efficient pest inhibitor; phenylacetaldehyde is also used in food additives, cosmetics and soaps, etc. aspect. At present, the common industrial production method of phenylacetaldehyde is to prepare phenylacetaldehyde by oxidation of phenylethyl alcohol or reduction of ethyl phenylacetate. Because phenylacetaldehyde is active in nature and easy to oxidize and polymerize, the current industrial method cannot obtain high yield and high purity. ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C45/58C07C47/228
CPCC07C45/58C07C45/41C07D301/02
Inventor 李风浪
Owner DONGGUAN LIANZHOU INTPROP OPERATION MANAGEMENT CO LTD
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