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Preparation method and purification method of watermelon ketone crude product suitable for industrial production

A purification method, watermelon ketone technology, applied in the field of synthesis of spice compounds, can solve the problems of increased material cost, complex process route, low distillate yield, etc., and achieve the effect of improving conversion rate, optimizing reaction, and simple reaction route

Active Publication Date: 2022-04-08
江苏恒沛药物科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The process route is complicated, the material cost increases, and the yield is low
[0021] According to CN200810244583.7 technology crude product is washed and distilled under reduced pressure, the yield of distillate is lower

Method used

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  • Preparation method and purification method of watermelon ketone crude product suitable for industrial production
  • Preparation method and purification method of watermelon ketone crude product suitable for industrial production
  • Preparation method and purification method of watermelon ketone crude product suitable for industrial production

Examples

Experimental program
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Effect test

Embodiment 1

[0062]Put 30.56g of 4-methylcatechol and 300ml of 2-butanone into a 500mL four-necked bottle, stir for 0.5h to dissolve. 6.13 g potassium iodide and 52.18 g sodium carbonate were added. Heat and stir to raise the temperature to 75-80°C. At this temperature, a solution of 37.5 g of 1,3-dichloroacetone in 60 ml of 2-butanone was slowly added dropwise. After 3 hours of the reaction, gas phase detection of 4-methylcatechol was taken to be consumed below 2.0%, and the reaction was stopped. After desalting by suction filtration, the filtrate was concentrated under reduced pressure to recover the solvent. The crude watermelon ketone obtained was beaten with 300ml of n-heptane at room temperature for 0.5h, and then left to stand and layered to remove tar. Add 2.5 g of activated carbon to the beating liquid, stir at room temperature for 0.5 h, and filter with suction, the filtrate is clear and bright. Concentrate under reduced pressure to recover n-heptane. The still liquid was di...

Embodiment 2

[0064] Put 30.56g of 4-methylcatechol and 300ml of 2-butanone into a 500mL four-necked bottle, stir for 0.5h to dissolve. 6.13 g potassium iodide and 52.18 g sodium carbonate were added. Heat and stir to raise the temperature to 75-80°C. At this temperature, a solution of 34.5 g of 1,3-dichloroacetone in 60 ml of 2-butanone was slowly added dropwise. After 3 hours of the reaction, gas phase detection of 4-methylcatechol was taken to be consumed below 2.0%, and the reaction was stopped. After desalting by suction filtration, the filtrate was concentrated under reduced pressure to recover the solvent. The crude watermelon ketone obtained was beaten with 280 ml of n-heptane at room temperature for 0.5 h, and then left to stand for layering to remove tar. Add 2.0 g of activated carbon to the beating liquid, stir at room temperature for 0.5 h, and filter with suction, the filtrate is clear and bright. Concentrate under reduced pressure to recover n-heptane. The still liquid wa...

Embodiment 3

[0066] Put 30.56g of 4-methylcatechol and 300ml of 2-butanone into a 500mL four-necked bottle, stir for 0.5h to dissolve. 6.13 g potassium iodide and 68.03 g potassium carbonate were added. Heat and stir to raise the temperature to 75-80°C. At this temperature, a solution of 37.5 g of 1,3-dichloroacetone in 60 ml of 2-butanone was slowly added dropwise. After 2 hours of reaction, gas phase detection of 4-methyl catechol consumption was taken to be below 2.0%, and the reaction was stopped. After desalting by suction filtration, the filtrate was concentrated under reduced pressure to recover the solvent. The crude watermelon ketone obtained was beaten with 300ml of n-heptane at room temperature for 0.5h, and then left to stand and layered to remove tar. Add 2.5 g of activated carbon to the beating liquid, stir at room temperature for 0.5 h, and filter with suction, the filtrate is clear and bright. Concentrate under reduced pressure to recover n-heptane. The still liquid wa...

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Abstract

The invention discloses a preparation method of a crude watermelon ketone product suitable for industrial production, and the crude watermelon ketone product is produced by reacting a 2-butanone solution of 4-methylcatechol with 1, 3-dichloroacetone. The reaction route is simple, and the conversion rate is improved. The invention also provides a purification method of the watermelon ketone crude product suitable for industrial production. The purification method comprises the following steps: (1) removing tar in the watermelon ketone crude product; (2) distilling the decoked crude product for primary purification; and (3) recrystallizing the distilled watermelon ketone crude product to obtain a solid watermelon ketone pure product. The method has the advantages of high purity and few impurities. And tar is removed from the crude watermelon ketone product, so that tar accumulation in the distillation process can be prevented from damaging the product and influencing crystallization of the product. The distillation yield is greatly improved. And a high-yield and high-purity pure watermelon ketone product can be obtained through recrystallization treatment.

Description

technical field [0001] The invention relates to a method for preparing and purifying crude watermelon ketone suitable for industrial production, and belongs to the technical field of synthesis of fragrance compounds. Background technique [0002] At present, the preparation method of synthetic watermelon ketone mainly contains five kinds: [0003] Method 1: CN108164499A [0004] [0005] R=-Br,-OTs,-OMs [0006] In this method, a ketal is first used to form a ring, and the raw material is not easy to obtain, and ether needs to be used for extraction in the second step. The solvent has a low boiling point and is used for anesthesia in medicine, so it is not suitable for industrial production; [0007] Method 2: U.S. Patents US3517031, US3647479, and Chinese Patent CN101962378 disclose the following methods: [0008] [0009] In the method, 4-methylcatechol and methyl bromoacetate are used as raw materials to synthesize dicarboxylate intermediates through Williamson r...

Claims

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Application Information

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IPC IPC(8): C07D321/10
CPCY02P20/10
Inventor 陆樊委祝勇杰蒋君康余龙冯亚兵吴正华
Owner 江苏恒沛药物科技有限公司
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