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Synthetic method for nicotinamide

A synthesis method and nicotinamide technology, applied in the field of chemistry, can solve problems such as the further improvement of selectivity, and achieve the effects of less three wastes, mild reaction conditions and high economy

Active Publication Date: 2018-08-17
NANJING REDSUN BIOCHEM CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Others, such as American Ventrus, India Jiyoulian and domestic Brother Technology, mainly use the ammonia oxidation method for production. The process is mature, but it also needs to be carried out at high temperature, and the selectivity of the subsequent cyanohydrolysis process needs to be further improved.

Method used

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  • Synthetic method for nicotinamide

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Add 18.8g of 3-picoline (0.2mol, purity 99%, water content 0.37%), absolute ethanol 47g in 100mL ordinary photochemical reactor, turn on the cooling circulation system, turn on the 420nm purple light lamp (power 10W), start to The flow rate of 4.8g / h is passed into nitrosyl chloride to form a good turbulence state in the reactor, the temperature control reaction temperature is between 15 and 18°C, the reaction is about 3h, and the qualitative raw material 3-picoline is converted in the middle control complete. Stop feeding nitrosyl chloride, switch to blowing nitrogen gas for 0.3h, slightly reduce the flow rate and add about 20g of sodium carbonate at the same time, adjust the pH to 7.6, stop ventilation, filter the precipitated sodium chloride 12g, and the filtrate is pyridine-3- 66 g of ethanol solution of formaldehyde oxime, the content of pyridine-3-formaldehyde oxime determined by liquid phase is 33.64%, and the molar yield is 90.95% based on 3-picoline.

[0030] ...

Embodiment 2

[0032] Add 3-picoline 103g (1.1mol, purity 99%, water content 0.42%), dehydrated ethanol 206g in 500mL ordinary photochemical reactor, turn on cooling circulation system, turn on 480nm blue light (power 30W), start with 20g The flow rate of / h is fed into nitrosyl chloride to make the liquid in the reactor form a better turbulent state. The temperature control reaction temperature is between 15 and 18 ° C. The reaction is about 4.5 hours, and the conversion of the qualitative raw material 3-picoline is completed. . Stop feeding nitrosyl chloride, switch to blowing nitrogen gas for 0.9h, slightly reduce the flow rate and add about 40g caustic soda, adjust the pH to 7.2, stop ventilation, filter the precipitated sodium chloride 68g, and the filtrate is pyridine-3- The ethanol solution of formaldehyde oxime is 360g, the content of pyridine-3-formaldehyde oxime is 34.72% as determined by liquid phase, and the molar yield is 93.44% based on 3-picoline.

[0033] Add 360g of the eth...

Embodiment 3

[0035] Add 3-picoline 188g (2mol, purity 99%, water content 0.29%), dehydrated ethanol 400g in 1000mL ordinary photochemical reactor, turn on cooling circulation system, turn on 540nm green light (power 90W), begin to use 30g The flow rate of / h is passed into nitrosyl chloride to make the liquid in the reactor form a better turbulent state. The temperature control reaction temperature is between 15 and 18 ° C. The reaction is about 5 hours, and the conversion of the qualitative raw material 3-picoline is completed. . Stop feeding nitrosyl chloride, switch to blowing nitrogen gas for 1.5h, slightly reduce the flow rate, and add about 150g of sodium bicarbonate solid at the same time, adjust the pH to 6.8, stop ventilation, filter 130g of precipitated salt, and obtain pyridine-3-carbaldehyde oxime 741g of ethanol solution, the content of pyridine-3-carbaldehyde oxime determined by liquid phase is 30.53%, based on 3-picoline, the molar yield is 92.66%.

[0036]Add 741g of the e...

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Abstract

The invention belongs to the field of organic chemistry, and discloses a synthetic method for nicotinamide. The method comprises the following steps: using ethanol as a solvent, using 3-methylpyridineas a raw material, introducing a dried nitrosyl chloride gas, performing a photonitrosation-isomerization reaction under irradiation of visible light at temperature of 0-30 DEG C, after the reactionis completed, introducing a nitrogen gas, adding an alkali to adjust pH of the reaction solution to be 6-9, and performing filtration to obtain a filtrate; and adding a copper salt and a nitrile intothe filtrate as a catalyst, performing heating, performing reflux, performing an aldoxime Beckmann rearrangement reaction, after the reaction is completed, adding ethyl acetate crystals into the reaction solution, performing filtration to obtain a crude product of the nicotinamide, and performing recrystallization on the crude product of the nicotinamide to obtain a pure product of the nicotinamide. The synthetic method provided by the invention has mild reaction conditions, a simple process and a high yield, can obtain the high-purity nicotinamide product, has less three waste (waste water, waster gas and solid waste) and high economy, and is suitable for industrialized large-scale production.

Description

technical field [0001] The invention belongs to the field of chemistry, and in particular relates to a method for synthesizing nicotinamide. Background technique [0002] Nicotinamide, also known as Nicotinamide, commonly known as VB 3 , chemical name is 3-pyridine carboxamide, CAS number is 98-92-0, white needle crystal or powder, soluble in water, ethanol and glycerin. [0003] Nicotinamide is one of the important components of coenzyme Ⅰ and coenzyme Ⅱ, etc. It participates in various redox reactions in the body, and is of great significance to the energy cycle in the organism and the metabolism of fat, protein and carbohydrates. It is widely used in feed, food, Daily chemical and pharmaceutical industries. Its physiological effect is similar to that of niacin, but its water solubility is better, and it has no obvious vasodilator effect. [0004] At present, there are many known methods for preparing nicotinamide, but there are actually only two methods with industrial...

Claims

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Application Information

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IPC IPC(8): C07D213/82
CPCC07D213/82
Inventor 占新华钟劲松王福军陈洪龙慕灯友杨成
Owner NANJING REDSUN BIOCHEM CO LTD
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