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A kind of preparation method of safrole

A safrole and temperature control technology, which is applied in the field of safrole preparation, can solve the problems that trimethylallylsilane is expensive and difficult to obtain, and industrialization is difficult to realize, and achieves the effects of less material, low production cost and environmental friendliness

Active Publication Date: 2015-12-09
浦杰香料(上海)有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

On the one hand, the raw material trimethylallylsilane used in this method is expensive and difficult to obtain; on the other hand, the particularity of the reaction process makes its industrialization difficult to realize

Method used

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Examples

Experimental program
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Effect test

Embodiment 1

[0029] A kind of preparation method of safrole, concrete steps are as follows:

[0030] Add 146.54g (1.2mol) of piperonylcycline and 2.33g (0.04mol) of allyl alcohol into a three-necked glass reactor equipped with a thermometer, a condenser tube, and a drying tube, and then add 14.65g of catalyst Nafion-H, and control the temperature as Carry out Friedel-Crafts reaction at 15-50°C with a stirring speed of 500-800r / min. During the reaction process, use the GC6890-MS5973 gas chromatograph of Aglient in the United States to detect the content of allyl alcohol. When the reaction of allyl alcohol is basically completed, that is, the Friedel-Crafts reaction is 4h After stopping the reaction, the reaction solution was obtained;

[0031] The amount of piperonyl ring and allyl alcohol used in the above-mentioned Friedel-Crafts reaction is calculated by molar ratio, that is, piperonyl ring: allyl alcohol is 30:1; the amount of catalyst Nafion-H used is calculated according to its mass w...

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PUM

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Abstract

The invention discloses a method for preparing safrole. The method comprises the following steps: by taking commercially available allyl alcohol and benzodioxole as raw materials and simultaneously taking benzodioxole as a solvent, controlling the temperature at 15-50 DEG C under the action of a catalyst Nafion-H; carrying out friedel-craft reaction for 6-10 hours at the agitating speed of 500-800r / min; and removing the benzodioxole solvent from a benzodioxole solution which is obtained from the prepared reaction solution in manners of filtering, washing and drying by reduced pressure distillation, and then carrying out column chromatography; finally obtaining the safrole. The method for preparing the safrole disclosed by the invention is simple in preparation process, low in production cost, and applicable to large-scale production. Furthermore, by adopting the method for preparing the safrole disclosed by the invention, the raw material benzodioxole for reaction can be recycled as the solvent, the catalyst Nafion-H also can be recycled, and the generated waste is less. Therefore, the method is friendly to environment.

Description

technical field [0001] The invention relates to a preparation method of safrole. Background technique [0002] Safrole, also known as safrole, is called Safrole in English. It is a colorless or light yellow liquid with a smell of camphor wood. Its structural formula is. Soluble in ethanol, miscible with chloroform and ether, insoluble in water and glycerin. The relative density is 1.096, the freezing point is about 11°C, the boiling point is 232-234°C, the refractive index is 1.538, and the flash point is 97°C. Safrole is the main component of many edible natural flavors such as sassafras essential oil, star anise essential oil and camphor oil, accounting for about 80% of sassafras essential oil. Safrole also has a small amount in flavors made of nutmeg, Japanese wild ginger, California laurel and other spices exist. Sassafras essential oil is often used as a flavor addition to beer and other alcohols. The root bark of the sassafras tree (Sas-safrasalbidum) is also the m...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D317/50
CPCC07D317/50
Inventor 欧文华
Owner 浦杰香料(上海)有限公司
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