Preparation method of watermelon ketone

A technology of watermelon ketone and dichloroacetone, which is applied in the direction of organic chemistry, can solve the problems of high price of watermelon ketone and complicated synthetic route, and achieve the effect of low cost, high product purity and low possibility
CN113248467AInactive Publication Date: 2021-08-13CENT SOUTH UNIV
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Patent Information

Authority / Receiving Office
CN · China
Current Assignee / Owner
CENT SOUTH UNIV
Publication Date
2021-08-13
Estimated Expiration
Not applicable · inactive patent

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Abstract

The invention relates to a preparation method of watermelon ketone, which comprises the following steps: by taking 4-methylcatechol and 1,3-dichloroacetone as raw materials and carbonate as a base catalyst, adding a drying agent into a Soxhlet extractor for dehydration, and under the protection of inert gas, assembling a reduced pressure reflux water removal device to prepare a watermelon ketone crude product; carrying out rotary evaporation to recover a solvent, carrying out post-treatment steps of decoloration, concentration and the like, and transferring an obtained solution into a rectification device provided with a glass vacuum rectification column to carry out segmented rectification: in first-stage rectification, evaporating off reaction solvent light components, in second-stage rectification, collecting fractions to obtain a residual raw material 4-methylcatechol and a part of crude product watermelon ketone, and in third-stage rectification, collecting a main fraction watermelon ketone crude product; and recrystallizing the watermelon ketone crude product. According to the preparation method of the watermelon ketone, the yield of the watermelon ketone is improved through the reduced pressure reflux water removal device, the watermelon ketone is purified step by step by combining segmented rectification and recrystallization, the purity of the product reaches 98% or above, the technological process is simplified, and the problem that industrial large-scale production is difficult to achieve through an existing watermelon ketone synthesis technology is solved.
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Description

technical field

[0001] The invention belongs to the technical field of synthesis of spice compounds, and in particular relates to a preparation method of watermelon ketone. Background technique

[0002] With the development of industrial society, people are doing more and more research on spices, and the application of spices is becoming more and more extensive, and people are increasingly inseparable from "perfuming". Perfume, also known as fragrance raw material, is a substance that can be detected by the sense of smell or taste. It was first expressed in English as 'perfume', which means to emit fragrance. The original source of fragrances is natural fragrances, almost all of which are mixtures. As people's demand for fragrances increases, natural fragrances can no longer meet people's needs for flavoring substances. With the development of organic chemistry, synthetic fragrances began to replace natural fragrances. Spices enter people's lives.

[0003] In 1966, Beerebo...

Claims

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