Method for synthesizing watermelon ketone

A technology of watermelon ketone and dichloroacetone, which is applied in the direction of organic chemistry, can solve the problems of complicated purification steps, undisclosed watermelon ketone purity, and chemical reactions involved, and achieve the effect of improving purity, good selectivity, and less side reactions

Active Publication Date: 2022-05-10
SHANDONG NHU PHARMA +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The purification steps of this method are complicated and involve chemical reactions. In addition, the patent does not specifically disclose the purity of the final watermelon ketone

Method used

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  • Method for synthesizing watermelon ketone
  • Method for synthesizing watermelon ketone
  • Method for synthesizing watermelon ketone

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0065] Add 20g of anion resin D301 to a fixed-bed reactor with an inner diameter of 12mm and a length of 40cm. The particle size of the anion resin is 10-20 mesh, it is filled from the bottom of the reactor, the filling height is 25cm, and the filling density is 0.7g / cm 3 . Under the protection of nitrogen, 4-methylcatechol and 1,3-dichloroacetone dissolved in benzophenone (the moles of 1,3-dichloroacetone and 4-methylcatechol than n 二氯 / n 二酚 1:1, the mass ratio m of benzophenone and 4-methylcatechol 溶剂 / m 二酚 0.5:1) into the fixed bed reactor, under normal pressure, at a space velocity of 1.0h -1 , The reaction was carried out under the condition that the reaction temperature was 110°C. The reaction solution was collected for a period of time (124 g of raw material 4-methylcatechol was introduced in total), and the watermelon ketone fraction was collected by rectification under reduced pressure, which was 173.3 g. The watermelon ketone cut that 173.3g collects is transf...

Embodiment 2

[0067] Add 20g of anion resin D301 to a fixed-bed reactor with an inner diameter of 12mm and a length of 40cm. The particle size of the anion resin is 10 to 20 mesh. Filling starts from the bottom of the reaction tube, the filling height is 25cm, and the filling density is 0.7g / cm 3 . Under the protection of nitrogen, 4-methylcatechol and 1,3-dichloroacetone dissolved in benzophenone (the moles of 1,3-dichloroacetone and 4-methylcatechol than n 二氯 / n 二酚 1:1, the mass ratio m of benzophenone and 4-methylcatechol 溶剂 / m 二酚 0.5:1) into the fixed bed reactor, under normal pressure, at a space velocity of 1.0h -1 , The reaction was carried out under the condition that the reaction temperature was 110°C. Collect the reaction solution for a period of time (a total of 124 g of raw material 4-methylcatechol was introduced), and rectify under reduced pressure to collect 173.3 g of the watermelon ketone fraction; transfer the watermelon ketone fraction to a two-necked bottle, add 200...

Embodiment 3-23

[0069] On the basis of Example 2, the reaction conditions were changed without changing the post-treatment separation method, and the purity and yield results are shown in Table 1. Each catalyst is operated for a long period, and after 1000 hours, the purity of the product watermelon ketone fluctuates by ±0.1%, and the yield fluctuates by ±0.2%, that is, the catalyst has good stability.

[0070] The reaction conditions and reaction result of table 1 watermelon ketone synthesis

[0071]

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Abstract

The invention discloses a method for synthesizing watermelon ketone. 4-methylcatechol and 1, 3-dichloroacetone are used as raw materials to react in an organic solvent to obtain the watermelon ketone, the reaction is carried out in the presence of a catalyst, and the catalyst is anion exchange resin. The boiling point of the organic solvent is 300-350 DEG C. The method further comprises recrystallization post-treatment combining dynamic recrystallization and traditional static recrystallization under stirring. The method is a one-step reaction, the used catalyst is high in reaction selectivity, the product yield and purity are high, and the fragrance of the product is not influenced.

Description

technical field [0001] The invention relates to a method for synthesizing watermelon ketone. Background technique [0002] Watermelon ketone, 7-methyl-3,4-dihydro-2H-1,5-benzodioxepin-3-one, foreign trade name Calone / Watermelon ketone, its structure is as follows: [0003] [0004] The appearance of watermelon ketone is a white powdery crystalline solid with a melting point of 37-41°C and a boiling point of 305°C. 1g of watermelon ketone is dissolved in 5mL of 95% ethanol. Watermelon ketone not only has a fresh, fruity, soft and sweet smell, but also has a marine, algae, and dreamy feeling. It is widely used in the fragrance of medicine, food, washing and other products. Watermelon ketone is a high value-added fine chemical, the market demand is increasing year by year, and the prospect is broad. [0005] At present, using 4-methylcatechol and dichloroacetone as raw materials to prepare watermelon ketone is one of its synthetic methods. [0006] Zhang Jing disclosed in...

Claims

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Application Information

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IPC IPC(8): C07D321/10
CPCC07D321/10Y02P20/584
Inventor 张玉霞马啸于明孙小青黄珊珊
Owner SHANDONG NHU PHARMA
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