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Method for preparing nicotinamide

A technology of nicotinamide and cyanopyridine, which is applied in the field of nicotinamide preparation, can solve problems such as the low pH value of nicotinamide products, difficulty in meeting requirements, and increased production costs, and achieve easy product separation, good product quality, and high production capacity. sufficient effect

Active Publication Date: 2010-10-06
浙江新赛科药业有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, these existing methods above all have some defects: although the conversion rate of 3-cyanopyridine is very high, the selectivity is very poor, and a part of by-product nicotinic acid will be produced in the reaction, so that the pH value of the obtained nicotinamide product is not high , it is difficult to meet the requirement
If you want to meet the requirements, you generally need to carry out multiple refining, so the yield will be relatively low, and the production cost will be greatly increased

Method used

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  • Method for preparing nicotinamide

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Effect test

Embodiment 1

[0026] The preparation of embodiment 1 nicotinamide

[0027] In a 1000ml four-necked flask, throw 20g (0.23mol) of manganese dioxide, 100g (0.96mol) of solid 3-cyanopyridine, and 400g of ethanol (wherein ethanol 380g, 8.25mol; water 20g) with a mass percentage concentration of 95%. , 1.11mol). Stir and heat up to 90°C to start heat preservation, keep the temperature at 90°C + 5°C for 6 hours and then end the reaction. After the reaction, the reaction product is sampled for detection by HPLC. Test results (HPLC): Based on the integral of the peak area normalization method, the mass percentage of nicotinamide was 99.7%, the mass percentage of nicotinic acid was 0.3%, and 3-cyanopyridine was not detected; the reaction conversion rate was 100%, Selectivity 99.7%. The reaction product was rotary evaporated to dryness, then taken out, and vacuum-dried at 60° C. for 10 hours to obtain 116.7 g of nicotinamide, the molar yield of nicotinamide was 99.49%, and the pH value was 7.0.

Embodiment 2

[0028] The preparation of embodiment 2 nicotinamide

[0029] In a 1000ml four-neck flask, put 20g (0.23mol) of manganese dioxide, 100g (0.96mol) of solid 3-cyanopyridine, 450g (6.07mol) of n-butanol and 22g (1.22mol) of water. Stir and heat up to 80°C and start to keep warm, keep the temperature at 80°C+7°C for 8 hours and then end the reaction. After the reaction, the reaction product is sampled and detected by HPLC. Test results (HPLC): Based on the integral of the peak area normalization method, the mass percentage of nicotinamide was 99.5%, the mass percentage of nicotinic acid was 0.5%, and 3-cyanopyridine was not detected; the reaction conversion rate was 100%, Selectivity 99.5%. The reaction product was rotary evaporated to dryness and then taken out. After vacuum drying at 80° C. for 16 hours, 116.9 g of nicotinamide was obtained. The molar yield of nicotinamide was 99.66%, and the pH value of nicotinamide was 6.9.

Embodiment 3

[0030] The preparation of embodiment 3 nicotinamide

[0031] In a 1000ml four-necked flask, throw 15g (0.173mol) of manganese dioxide, 100g (0.96mol) of solid 3-cyanopyridine, 300g (9.36mol) of methanol, and 18g (1.00mol) of water. Stir and heat up to 95°C to start heat preservation, keep the temperature at 95°C ± 5°C for 7 hours and then end the reaction. After the reaction, the reaction product is sampled for detection by HPLC. Test results (HPLC): Based on the integral of the peak area normalization method, the mass percentage of nicotinamide was 99.4%, the mass percentage of nicotinic acid was 0.6%, and 3-cyanopyridine was not detected; the reaction conversion rate was 100%, Selectivity 99.4%. The reaction product was rotary evaporated to dryness, then taken out, and vacuum-dried at 70° C. for 8 hours to obtain 116.5 g of nicotinamide, the molar yield of nicotinamide was 99.32%, and the pH value was 6.8.

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Abstract

The invention discloses a method for preparing nicotinamide, which comprises the following steps: dissolving 3-cyanopyridine in alcohol; adding water and a catalyst to perform a hydrolysis reaction; and performing posttreatment on the reaction product to obtain the nicotinamide. The method avoids introducing auxiliary reagents, is highly economic, ensures mild reaction conditions, easy product separation, high product purity and high yield, generates little waste gas, liquid and solid, and is favorable for industrial production.

Description

technical field [0001] The invention belongs to the field of medicinal chemistry, and in particular relates to a preparation method of nicotinamide. Background technique [0002] Currently, there are many ways to convert cyanopyridines to amides, both chemically and biologically. Both Japanese Patent JP93-206579 and European Patent EP85-306670 disclose the use of modified Raney nickel catalysts for the conversion of cyanopyridines into amides. WO90 / 09988Al discloses the use of alkali metal borates for the conversion of cyanopyridines into amides. US Patent No. 2,471,518, US Patent No. 4,721,709, and German Patent Application DE 2,517,054 all disclose the hydrolysis of 3-cyanopyridine in the presence of sodium hydroxide. [0003] Niacinamide is divided into pharmaceutical grade and feed grade products. According to the current version of the Chinese Pharmacopoeia, the pH value range of pharmaceutical grade products is 5.5-7.5, and the pH value of high-grade nicotinamide is ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D213/82
Inventor 华宇宁何勇陆能勇黄飞喜吕士华郭拥政杨和军
Owner 浙江新赛科药业有限公司
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