A kind of method utilizing carbon dioxide to synthesize nicotinic acid

A technology of carbon dioxide and nicotinic acid, applied in the direction of organic chemistry, can solve the problems of increased equipment investment, low product purity, three waste pollution, etc., and achieve the effect of convenient operation, simple process and high conversion rate

Active Publication Date: 2021-01-12
HUNAN XIANGYIKANG PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, in terms of economy and technology, these methods have certain deficiencies: although the direct reagent oxidation method is simple to operate and has a wide range of oxidant sources, it generally requires higher temperature or pressure, low product purity, poor color, and serious pollution of three wastes. Developed countries have eliminated this method
The obvious disadvantage of the ammoxidation method is that the product obtained from the raw material alkylpyridine requires at least two independent chemical reactions, which increases the investment in equipment.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] In a 150 mL stainless steel autoclave, add 3.16 g of 3-bromopyridine, 36.86 g of ethanol, 0.26 g of palladium acetate and 0.06 g of diethyl zinc complex catalyst. After the reactor was sealed, it was filled with carbon dioxide with a purity of 5 Mpa and 99.9%. Under the condition of the magnetic sub-rotational speed of 180 r / min, the temperature controller controlled the temperature program to raise the temperature to 200 °C, reacted for 3 hours, and cooled to room temperature. The gas in the tank was controlled by pressure. The valve slowly drains the reactor and absorbs it with ethanol solvent. After the gas in the kettle is released, open the kettle to collect the reaction liquid and absorption liquid, put them in a distillation bottle and carry out vacuum distillation at about 105 °C until it is nearly evaporated to dryness, and the distilled part is carried out. Condensation and recovery for recycling; pyridine is completely removed by vacuum distillation, but the e...

Embodiment 2

[0020] In a 150 mL stainless steel autoclave, 3.16 g of 3-bromopyridine, 36.86 g of ethanol, 0.26 g of nickel acetate and 0.06 g of diethylzinc complex catalyst were added. After the reactor was sealed, it was filled with carbon dioxide with a purity of 5 Mpa and 99.9%. Under the condition of the magnetic sub-rotational speed of 180 r / min, the temperature controller controlled the temperature program to raise the temperature to 200 °C, reacted for 3 hours, and cooled to room temperature. The gas in the tank was controlled by pressure. The valve slowly drains the reactor and absorbs it with ethanol solvent. After the gas in the kettle is released, open the kettle to collect the reaction liquid and absorption liquid, put them in a distillation bottle and carry out vacuum distillation at about 105 °C until it is nearly evaporated to dryness, and the distilled part is carried out. Condensation and recovery for recycling; pyridine is completely removed by vacuum distillation, but th...

Embodiment 3

[0022] In a 150 mL stainless steel autoclave, add 6.32 g of 3-bromopyridine, 36.86 g of ethanol, and add 0.26 g of palladium acetate and 0.06 g of diethyl zinc composite catalyst. After the reactor was sealed, it was filled with carbon dioxide with a purity of 5 Mpa and 99.9%. Under the condition of the magnetic sub-rotational speed of 180 r / min, the temperature controller controlled the temperature program to raise the temperature to 200 °C, reacted for 3 hours, and cooled to room temperature. The gas in the tank was controlled by pressure. The valve slowly drains the reactor and absorbs it with ethanol solvent. After the gas in the kettle is released, open the kettle to collect the reaction liquid and absorption liquid, put them in a distillation bottle and carry out vacuum distillation at about 105 °C until it is nearly evaporated to dryness, and the distilled part is carried out. Condensation and recovery for recycling; pyridine is completely removed by vacuum distillation,...

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Abstract

The invention discloses a new method for synthesizing nicotinic acid by utilizing carbon dioxide, belonging to the field of organic chemical synthesis, using 3-halopyridines, carbon dioxide as raw materials, and ethanol as a solvent to directly prepare nicotinic acid under the action of a catalyst; the characteristics of the catalyst The active component of the catalyst is composed of palladium acetate and diethyl zinc, the catalyst dosage is 3-bromopyridine:catalyst=20:1~2 weight ratio, the reaction temperature is 100~250℃, the reaction pressure is 1~10 MPa, the reaction The time is 1 to 5 hours; the present invention uses carbon dioxide directly as a chemical raw material to synthesize chemicals, which is the most important and more valuable way to utilize carbon dioxide, and the yield and selectivity of the target product are high, which is beneficial to reduce niacin The production cost is low, and it has good industrial application value.

Description

technical field [0001] The invention relates to the synthesis of nicotinic acid, in particular to a method for preparing nicotinic acid in the presence of a catalyst by using 3-halopyridine and carbon dioxide as raw materials and ethanol as a solvent, belonging to the technical field of organic chemical synthesis. Background technique [0002] Nicotinic acid, that is, pyridine-3-carboxylic acid, also known as nicotinic acid, referred to as VB 3 , the molecular formula is: C 6 h 5 NO 2 , the structural formula is: , Molecular weight 123.11, white or light yellow needle crystal or powder, odorless or slightly smelly, slightly sour taste. Density 1.4738 g / cm3, melting point 234~238 ℃. Stable in the air, and not hygroscopic, the aqueous solution is acidic. Slightly soluble in water, easily soluble in boiling water, boiling ethanol and sodium hydroxide solution. Niacin combines with protein in the body to form a coenzyme, which participates in the oxidation and reduction ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D213/80
CPCC07D213/80
Inventor 帅放文王向峰章家伟
Owner HUNAN XIANGYIKANG PHARMA
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