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Method for synthesizing compound in condensed carbonyl group

A technology of carbonyl compounds and synthesis methods, applied in the field of synthesis of organic compounds, can solve the problems of not being suitable for industrial scale production and use, difficulties in storage and handling, complex catalyst structures, etc., and achieve easy industrial production, easy acquisition, and short reaction time Effect

Inactive Publication Date: 2006-09-27
广州百花香料股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Sterzycki, R. (Synthesis, 1979, 724) has solved these problems with neutral catalyst p-pyridinium methylsulfonate, but this catalyst is very susceptible to moisture, and it is difficult to preserve and handle
Sang-Bong Lee et al. (Synthesis, 1991, 368) proposed to use N-benzylpyridinium salt as a catalyst with a yield of 85-95%. Complex structure, high manufacturing cost, not suitable for industrial scale production

Method used

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  • Method for synthesizing compound in condensed carbonyl group
  • Method for synthesizing compound in condensed carbonyl group

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0013] In a 500ml three-necked flask equipped with a heating mantle, a stirrer, a thermometer, and a reflux dehydration device, 100 g of neopentyl glycol, 167 g of acetophenone, 60 g of cyclohexane, and 0.5 g of alum were added. Turn on heating and stirring, keep the temperature at 115-118°C, reflux for 4 hours for dehydration reaction, and dehydrate 17.5g. After the reaction is completed, the reactant is cooled to room temperature, washed with brine three times, each time 200ml, the crude product is subjected to vacuum fractionation after removing the solvent, and the fraction at 98~100℃ / 0.1KPa is collected to obtain acetophenone neopentyl glycol ketal The product is 174.2g, calculated by neopentyl glycol, the product yield is 88.0%, and the product content is 98.5%. The product has woody, sandalwood and sweet fragrance, and the fragrance is pure.

Embodiment 2

[0015] In a 500ml three-neck flask equipped with a heating mantle, a stirrer, a thermometer, and a reflux dehydration device, 100 g of neopentyl glycol, 167 g of acetophenone, 60 g of cyclohexane, and 2.0 g of alum were added. Turn on heating and stirring, keep the temperature at 115-118°C, reflux dehydration reaction for 4 hours, and dehydrate 17.8g. After the reaction is completed, the reactant is cooled to room temperature, washed with brine three times, each time 200ml, the crude product is subjected to vacuum fractionation after removing the solvent, and the fraction at 98~100℃ / 0.1KPa is collected to obtain acetophenone neopentyl glycol ketal The product is 176.8g, calculated by neopentyl glycol, the product yield is 89.3%, and the product content is 98.8%. The product has woody, sandalwood and sweet fragrance, and the fragrance is pure.

Embodiment 3

[0017] In a 500ml three-necked flask equipped with a heating mantle, a stirrer, a thermometer, and a reflux dehydration device, 100 g of neopentyl glycol, 167 g of acetophenone, 60 g of cyclohexane, and 4.0 g of alum were added. Turn on heating and stirring, keep the temperature at 115-118°C, reflux for 6 hours for dehydration reaction, and dehydrate 18.5g. After the reaction is completed, the reactant is cooled to room temperature, washed with brine three times, each time 200ml, the crude product is subjected to vacuum fractionation after removing the solvent, and the fraction at 98~100℃ / 0.1KPa is collected to obtain acetophenone neopentyl glycol ketal The product is 178.5g, calculated by neopentyl glycol, the product yield is 90.2%, and the product content is 98.0%. The product has woody, sandalwood and sweet fragrance, and the fragrance is pure.

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Abstract

This invention relates method for synthesis of condensated carbonyl compound. Raw material alcohol and carbonyl compound, in molar ratio of (1:2)-(2:1), are reacted, in the presence of catalyst of white alum and organic solvent cyclohexane, at temp. 90-130 deg.C, heating and refuxing for 4-6 hrs. Advantages are; short reaction time, high yield, less side reaction, simple after-treatment of product, no corrosion, available catalyst, and commercialization prodn.

Description

technical field [0001] The invention relates to a method for synthesizing organic compounds, in particular to a method for synthesizing acetal compound spices. Background technique [0002] Carbonyl compounds are widely used in the perfume industry, and its synthetic method is usually to use corresponding carbonyl compounds and corresponding alcohols to reflux dehydration under acidic catalysts to obtain corresponding carbonyl compounds (Meskens, F.A.J.Synthesis, 1981,501 ). Due to the use of acidic catalysts in this method, production equipment will be corroded in industrial production. In the post-treatment process of the product, alkali needs to be used to neutralize the reaction product, which increases the post-treatment steps and production costs, and this method is suitable for those sensitive to acid. carbonyl compounds are not applicable. Sterzycki, R. (Synthesis, 1979, 724) solved these problems with neutral catalyst p-pyridinium methylsulfonate, but this catalys...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D325/00C07D317/10C07D319/06
Inventor 吴奇林甄宏爝钟炼军杨浩波张建斌
Owner 广州百花香料股份有限公司