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New method for synthesizing dietary supplement melatonin

A technology for dietary supplements and melatonin, applied in food science, organic chemistry and other directions, can solve the problems of complex synthesis process of melatonin, many chemical raw materials and high cost, and achieve easy industrial production, simple synthesis process and cost saving Effect

Active Publication Date: 2021-09-17
河北维达康生物科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] The present invention is proposed in view of the current complex synthesis process of melatonin, the use of many chemical raw materials and the low cost of the yield. The method of the present invention uses N-acetyl serotonin as the starting material, and obtains melatonin through a one-step methylation reaction. The synthetic process is simple, the synthetic process conditions are mild, the yield is as high as 98.5%, the quality is good, the content is greater than 99.5%, and it fully meets the USP42 standard

Method used

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  • New method for synthesizing dietary supplement melatonin

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Effect test

Embodiment 1

[0022] Under nitrogen protection, 21.8 g of N-acetyl serotonin was added into a 150 ml flask, then 88 g of 15% ethanol aqueous solution was added, and 100 mg of catalyst cetyltributylammonium bromide was added, and the mixture was stirred for 10 min. Then dropwise add 30% sodium hydroxide solution and dimethyl sulfate 14.49g at the same time, control the dropwise addition temperature at 20-23°C, keep the reaction system pH=11-11.3 during the dropwise addition process, dropwise time 30min, after the dropwise addition is completed , keep the temperature at 20-23°C and continue to react for 4h, take a sample to control the test, the remaining amount of N-acetyl serotonin is 0.09g / kg, then add 20% dilute sulfuric acid to the system to neutralize the system to pH=6.5. Turn on the vacuum, keep the vacuum degree from -0.095 to -0.097Mpa, set the temperature of the water bath at 60-70°C, and distill ethanol water under reduced pressure. When the distillation gas phase temperature reach...

Embodiment 2

[0024] Under nitrogen atmosphere, 21.8 g of N-acetylserotonin was added into a 150 ml flask, then 95 g of 15% ethanol aqueous solution was added, and 130 mg of catalyst benzyltrimethylammonium chloride was added, and the mixture was stirred for 10 min. Then dropwise add 30% sodium hydroxide solution and dimethyl sulfate 15.12g at the same time, control the dropwise addition temperature at 22-25°C, keep the reaction system pH=11.1-11.5 during the dropwise addition process, dropwise time 30min, after the dropwise addition is completed , keep the temperature at 20-25°C and continue to react for 3.5h, take samples for central control detection, the remaining amount of N-acetyl serotonin is 0.1g / kg, then add 20% dilute sulfuric acid to the system to neutralize the system to pH=6.2. Turn on the vacuum, keep the vacuum degree from -0.095 to -0.097Mpa, set the temperature of the water bath at 60-70°C, and distill ethanol water under reduced pressure. When the distillation gas phase tem...

Embodiment 3

[0026] Under a nitrogen atmosphere, 21.8 g of N-acetyl serotonin was added to a 150 ml flask, then 105 g of 15% ethanol aqueous solution was added, and the catalyst cetyltributylammonium bromide 66 mg was added, and the mixture was stirred for 10 min. Then dropwise add 30% sodium hydroxide solution and dimethyl sulfate 14.12g at the same time, control the dropwise addition temperature at 20-25°C, keep the reaction system pH=11.0-11.5 during the dropwise addition, dropwise time 30min, after the dropwise addition is completed , keep the temperature at 20-25°C and continue to react for 4 hours, take samples for central control detection, the remaining amount of N-acetyl serotonin is less than 0.1g / kg, then add 20% dilute sulfuric acid to the system to neutralize the system to pH=6.4. Turn on the vacuum, keep the vacuum degree from -0.095 to -0.097Mpa, set the temperature of the water bath at 60-70°C, and distill ethanol water under reduced pressure. When the distillation gas phase...

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Abstract

The invention discloses a novel method for synthesizing a dietary supplement melatonin, and belongs to the technical field of pharmaceutical chemical synthesis. According to the method, N-acetyl serotonin is used as a starting raw material, melatonin is obtained through one-step methylation reaction, the synthesis process is simple, the synthesis process conditions are mild, the yield is as high as 98.5% or above, the quality is good, the content is larger than 99.5%, and the melatonin completely meets the USP42 standard. The new method for synthesizing the dietary supplement melatonin provided by the invention saves the cost and is easy for industrial production.

Description

technical field [0001] The invention belongs to the technical field of pharmaceutical chemical synthesis, and in particular relates to a new method for synthesizing dietary supplement melatonin. Background technique [0002] Melatonin, also known as melatonin, its chemical name is N-acetyl-5-methoxytryptamine. Melatonin is an indole hormone secreted by the pineal gland of the human brain. Its main function is to maintain The circadian rhythm of the human body's own circadian rhythm is conducive to sleep. It can enhance the immune function of the human body and inhibit the growth of tumor cells. Melatonin may also have an inhibitory effect on the central nervous system; it is a more effective peroxide radical scavenger than vitamin E In addition, it regulates growth and development, sexual function and many organs. [0003] There are different processes for the synthesis of melatonin. At present, there are two main process routes: [0004] 1. Obtain 5-methoxytryptamine thro...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D209/14A23L33/10
CPCC07D209/14A23L33/10A23V2002/00A23V2200/30A23V2200/31
Inventor 李迁邵泉杨志彬崔金旺邢瑞静贾博硕张犇
Owner 河北维达康生物科技有限公司
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