Synthesis of 3-phenyl-2,3-epoxy sodium epihydrate

A technology of sodium glycidate and a synthesis method, applied in the direction of organic chemistry and the like, can solve the problems such as easy occurrence of side reactions and reduced reaction yield, and achieve the effects of increasing reaction yield and reducing polymerization reaction.

Inactive Publication Date: 2004-12-08
上海香料研究所
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Problems solved by technology

Natural cinnamaldehyde is an α, β unsaturated aldehyde with a phenyl group. It is easy to have side reactions by using the ordinary reaction method of oxidizing α, β unsaturated aldehydes, and many polymers are produced to reduce the reaction yield.

Method used

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  • Synthesis of 3-phenyl-2,3-epoxy sodium epihydrate

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Embodiment Construction

[0008] Further illustrate the implementation of the present invention below:

[0009] The natural cinnamon oil is separated by a high-efficiency rectification tower to obtain natural cinnamaldehyde with a content greater than 99%, which meets the requirements of flavoring grade, and then oxidizes natural cinnamaldehyde with an oxidant under freezing and catalytic conditions to obtain 3-phenyl-2, Sodium 3-epoxypropionate.

[0010] Add 318 grams (3mol) of anhydrous sodium carbonate, 100ml water, 400ml acetic acid, 264 grams (2mol) of 99% natural cinnamaldehyde in the 2000ml there-necked flask that stirrer, balanced type dropping funnel, interior thermometer are housed, open stirring , with CaCl 2 Cool the reaction solution with brine to reduce the reaction solution to -15°C, add 760 grams of 20% peracetic acid dropwise, the internal temperature does not exceed -5°C, the dropwise addition is completed in about 5 hours, and then keep at -5°C for 5 hours. Stop stirring, filter to...

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Abstract

A process for preparing 3-phenyl-2,3-sodium epoxy propionate features that under freezing condition and existance of catalyst chosen from sodium carbonate and sodium acetate, the cinnamaldehyde is oxidized by the oxidant chosen from ethaneperoxoic acid, peroxybenzoic acid and H2O2 at -15-40 deg.C for 5-15 hr to obtain product. Its advantages are low cost and low reaction temp.

Description

Technical field: [0001] The invention relates to a method for synthesizing raw materials for synthesizing natural grade phenylacetaldehyde fragrance. Background technique: [0002] Sodium 3-phenyl-2,3-epoxypropionate is the raw material for the synthesis of natural grade phenylacetaldehyde fragrance. Sodium 3-phenyl-2,3-epoxypropionate is synthesized by utilizing natural cinnamaldehyde, which is one of the unique bulk forest resources in my country and accounts for about 80% of the world's output. Natural cinnamaldehyde is an α, β unsaturated aldehyde with a phenyl group, and it is easy to have side reactions by using the common reaction method of oxidizing α, β unsaturated aldehydes, and many polymers are produced to reduce the reaction yield. Invention content: [0003] The present invention aims at the shortcoming of prior art, provides a kind of synthetic method of improved 3-phenyl-2,3-epoxypropionate sodium, has obtained the 3-phenyl-2 of higher yield, 3-cyclo Sodi...

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D303/38
Inventor 何锡敏
Owner 上海香料研究所
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