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Continuous synthesis method of piroctone

A technology of piroctone and chemical synthesis, applied in the direction of organic chemistry, can solve the problems of reduced process safety, oxidation failure, long reaction time, etc., and achieve the effects of reduced loss, process safety, and simple post-treatment process

Active Publication Date: 2020-04-07
湖南华腾医药有限公司
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Problems solved by technology

[0004] Because the method adopts the kettle-type intermittent synthesis process, the reaction time is longer and the product yield is lower, and the materials are added in batches in order. The contact time between the hydroxylamine hydrochloride solid and the air is too long, and it is easy to deliquesce or oxidize. As a result, by-products are produced, the difficulty of post-processing is increased, and the process safety will be greatly reduced.

Method used

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Examples

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preparation example Construction

[0024] The continuous synthetic method of the piroctone of one embodiment, comprises the following steps:

[0025] S110, providing a first solution, the first solution including 4-methyl-6-(2,4,4-trimethylpentyl)-2H-pyran-2-one, potassium tert-butoxide and isopropanol .

[0026] Wherein, the mass content of 4-methyl-6-(2,4,4-trimethylpentyl)-2H-pyran-2-one in the first solution is 10% to 30%, potassium tert-butoxide The mass content is 5% to 20%.

[0027] Prepare a homogeneous liquid system by mixing 4-methyl-6-(2,4,4-trimethylpentyl)-2H-pyran-2-one, potassium tert-butoxide and isopropanol to Ensure the fluidity of potassium tert-butoxide and raw materials, improve the reaction and catalytic effect.

[0028] S120. Provide a second solution, where the second solution includes hydroxylamine, water and isopropanol.

[0029] Wherein, the mass content of hydroxylamine in the second solution is 10%-30%, and the mass content of water is 5%-20%.

[0030] A homogeneous liquid syst...

Embodiment 1

[0050] Use two advection pumps (model MPF0502C, Shanghai Sanwei Scientific Instrument Co., Ltd.) to control the output of the first solution and the second solution, so that the first solution and the second solution are simultaneously pumped into the first solution inlet and the second solution of the microreactor. Inlet, contacts and initiates the hydroxylamination reaction in the microreactor.

[0051] Among them, the microreactor:

[0052] Model RMCS101010, Shandong Haomai Machinery Manufacturing Co., Ltd.

[0053] MaterialSiC

[0054] Hydraulic diameter 1mm

[0055] Reaction pipeline liquid holding capacity: 17.2ml

[0056] Process conditions:

[0057] In the first solution, 4-methyl-6-(2,4,4-trimethylpentyl)-2H-pyran-2-one 12wt.%, potassium tert-butoxide 12wt.%, isopropanol 66wt. %;

[0058] Hydroxylamine 30wt.% in the second solution, water 10wt.%, isopropanol 60wt.%;

[0059] The temperature of the microreactor is controlled at 150°C;

[0060] Reaction pressure...

Embodiment 2

[0073] Embodiment 2, reaction temperature changes in the microreactor

[0074] According to the same method as in Example 1, the reaction temperature in the microreactor was changed to 140° C., and other experimental conditions and analysis methods were the same as in Example 1. Implementation results: piroctone yield 85.1%, others 14.9%, raw material 4-methyl-6-(2,4,4-trimethylpentyl)-2H-pyran-2-one 0.

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Abstract

The invention relates to a continuous synthesis method of piroctone. The method comprises the following steps: providing a first solution and a second solution; and respectively and continuously pumping the first solution and the second solution into a microreactor, and reacting at the temperature of 90-180 DEG C and the pressure of 0.2-2MPa to obtain the piroctone. According to the synthesis method of the piroctone, potassium tert-butoxide is used as a catalyst and an alkali, isopropanol is used as a solvent, and a continuous synthesis process is realized by adopting the microreactor, so thatthe yield of the piroctone can reach more than 85%, the reaction time is shortened to be within 60 minutes, and the production cycle is shortened. Besides, the microreactor system is closed, so thatcontact reaction between hydroxylamine and oxygen, moisture and the like in the external environment is avoided, side reaction and loss of the hydroxylamine are greatly reduced, and the post-treatmentprocess is simpler and safer.

Description

technical field [0001] The invention relates to a micro-reaction synthesis method, in particular to a continuous synthesis method of piroctone. Background technique [0002] Piroctone, CAS No. 50650-76-5, Chinese alias 1-hydroxy-4-methyl-6-(2,4,4-trimethylpentyl)-2(1H)-pyridone, is a production The key material of piroctone olamine salt. Piroctone olamine salt is a highly effective, non-toxic and non-irritating anti-dandruff agent, which can be well mixed with other additives in shampoos, and is widely used in anti-dandruff shampoos, hair nourishing liquids and hair conditioners, etc. In washing and care cosmetics. [0003] The synthetic method of traditional piroctone is to use 3,5,5-trimethylhexanoic acid as the starting material, and the four-step method is used to synthesize piroctone, and one of the key steps is to use 4-methyl-6- (2,4,4-Trimethylpentyl)-2-pyrone was hydroxylated to synthesize piroctone. The hydroxylamination reaction of this step is to add the star...

Claims

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Application Information

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IPC IPC(8): C07D213/89
CPCC07D213/89Y02P20/55
Inventor 陈毅征陈仔玲许慧彭媛媛
Owner 湖南华腾医药有限公司
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