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

Inactive Publication Date: 2021-08-13
CENT SOUTH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The raw materials of this route are basic industrial raw materials, which are cheap and easy to get, but the synthetic route is complicated
[0011] At present, the synthesis of watermelon ketone is limite

Method used

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  • Preparation method of watermelon ketone
  • Preparation method of watermelon ketone
  • Preparation method of watermelon ketone

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0073] A kind of preparation method of watermelon ketone of the present embodiment, comprises the following steps:

[0074] 1) Assemble the decompression reflux water removal device

[0075] refer to figure 1, Assemble the decompression reflux water removal device according to the figure, and add anhydrous calcium chloride wrapped in filter paper into the Soxhlet extractor.

[0076] The key of the decompression reflux water removal device is to reduce the boiling point of water through decompression, distill the water out of the reaction system, and absorb it through the desiccant;

[0077] 2) Preparation of watermelon ketone reaction solution

[0078] Add 400.0mL of acetone to the 1000.0mL four-necked flask of the decompression reflux dewatering device, then add sodium carbonate (36.0g, 340.0mmol), add catalyst potassium iodide (4.0g, 24.0mmol); start mechanical stirring, and heat up to 45 ℃; Prepare 100.0 g (mass content of 29.8%) of 4-methylcatechol (29.8 g, 240.0 mmol) ...

Embodiment 2

[0094] A kind of preparation method of watermelon ketone of the present embodiment, comprises the following steps:

[0095] 1) Assemble the decompression reflux water removal device

[0096] refer to figure 1 , Assemble the decompression reflux water removal device according to the figure, and add anhydrous magnesium sulfate desiccant wrapped in filter paper into the Soxhlet extractor.

[0097] The key of the decompression reflux water removal device is to reduce the boiling point of water through decompression, distill the water out of the reaction system, and absorb it through the desiccant;

[0098] 2) Preparation of watermelon ketone reaction solution

[0099] Drop into 400mL of acetone in the 1000mL four-necked flask of the decompression reflux dewatering device, then add potassium carbonate (47g, 340.0mmol), add the catalyst potassium iodide (4.0g, 24.0mmol), start the mechanical stirring, heat up to 45°C, use Acetone is solvent preparation 4-methylcatechol (29.8g, 24...

Embodiment 3

[0110] A kind of preparation method of watermelon ketone of the present embodiment, comprises the following steps:

[0111] 1) Assemble the decompression reflux water removal device

[0112] refer to figure 1 , Assemble the decompression reflux water removal device according to the figure, and add anhydrous calcium chloride wrapped in filter paper into the Soxhlet extractor.

[0113] The key of the decompression reflux water removal device is to reduce the boiling point of water through decompression, distill the water out of the reaction system, and absorb it through the desiccant;

[0114] 2) Preparation of watermelon ketone reaction solution

[0115]Put 400 mL of acetone into a 1000 mL four-necked flask of a decompression reflux water removal device, then add sodium carbonate (36.0 g, 340.0 mmol), and add catalyst potassium iodide (4.0 g, 24.0 mmol). Turn on the mechanical stirring and raise the temperature to 45°C. Prepare 4-methylcatechol (29.8g, 240.0mmol) solution 1...

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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.

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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Application Information

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IPC IPC(8): C07D321/10
CPCC07D321/10
Inventor 蒋历辉余杰坤江佳红邹应萍
Owner CENT SOUTH UNIV
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