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2-pyridinemethanol and synthetic method thereof

A technology of pyridinemethanol and synthesis method, which is applied in chemical recovery, organic chemistry, etc., can solve the problems of high reaction pressure of catalytic hydrogenation, unsuitability for large-scale industrial production, and unsuitability for industrial production, so as to achieve difficult deactivation phenomenon, simplify Synthetic production steps, the effect of improving the conversion rate

Inactive Publication Date: 2015-12-16
ANHUI COSTAR BIOCHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The synthesis method of 2-pyridinemethanol is divided according to the starting materials used, mainly including the two routes of halogenation method and catalytic hydrogenation method. The reaction conditions of the halogenation method are harsh, difficult to control, and the production cost is high, so it is not suitable for Large-scale industrial production; the reaction pressure of catalytic hydrogenation method is high, the amount of catalyst is large, the reaction time is long, and the yield is low, so it is not suitable for industrial production

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] In a 3000L enamel glass reaction kettle, add 310Kg 2-picoline, 930kg glacial acetic acid, 3.0kg molybdenum trioxide, after stirring for 20-40 minutes, add 753.7Kg30% H2O2 dropwise at a temperature of 75°C, react for 3-5h, Cool down to normal temperature, filter the catalyst, and then distill the filtrate under reduced pressure to recover water and glacial acetic acid, extract the mother liquor with 600L of dichloromethane, separate liquid, and precipitate to obtain 2-picoline nitrogen oxide. Add 2-picoline nitrogen oxide to 862.5Kg acetic anhydride, and react under reflux for 3-6 hours. After the reaction is completed, glacial acetic acid and acetic anhydride are removed by rotary evaporation. The mother liquor is adjusted to pH 10 with powdered potassium carbonate, filtered, and the mother liquor Extract with 600L of dichloromethane, separate liquid, and desolventize to obtain acetic acid-2-picolyl methyl ester. Add 2-pyridinemethyl acetate into 500Kg of 20% NaOH solut...

Embodiment 2

[0024] In a 3000L enamel glass reactor, add 310Kg 2-picoline, 930kg glacial acetic acid, 1.6kg molybdenum trioxide, after stirring for 20-40 minutes, add 753.7Kg30% H2O2 dropwise at a temperature of 75°C, and react for 3-5h. Cool down to normal temperature, filter the catalyst, and then distill the filtrate under reduced pressure to recover water and glacial acetic acid, extract the mother liquor with 600L dichloroethane, separate liquid, and precipitate to obtain 2-picoline nitrogen oxide. Add 2-picoline nitrogen oxide to 862.5Kg acetic anhydride, and react under reflux for 3-6 hours. After the reaction is completed, glacial acetic acid and acetic anhydride are removed by rotary evaporation. The mother liquor is adjusted to pH 10 with powdered potassium carbonate, filtered, and the mother liquor Extract with 600L of dichloromethane, separate liquid, and desolventize to obtain acetic acid-2-picolyl methyl ester. Add 2-pyridinemethyl acetate into 500Kg of 20% NaOH solution, rea...

Embodiment 3

[0026] In a 3000L enamel glass reaction kettle, add 310Kg 2-picoline, 1240kg glacial acetic acid, 3.0kg molybdenum trioxide, stir for 20-40 minutes, then add 753.7Kg30% H2O2 dropwise at 75°C, react for 3-5h, Cool down to normal temperature, filter the catalyst, and then distill the filtrate under reduced pressure to recover water and glacial acetic acid, extract the mother liquor with 600L chloroform, separate liquid, and precipitate to obtain 2-picoline nitrogen oxide. Add 2-picoline nitrogen oxide to 862.5Kg acetic anhydride, and react under reflux for 3-6 hours. After the reaction is completed, glacial acetic acid and acetic anhydride are removed by rotary evaporation. The mother liquor is adjusted to pH 10 with powdered potassium carbonate, filtered, and the mother liquor Extract with 600L of dichloromethane, separate liquid, and desolventize to obtain acetic acid-2-picolyl methyl ester. Add 2-pyridinemethyl acetate into 500Kg of 20% NaOH solution, react for 2-4 hours unde...

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Abstract

The invention discloses 2-pyridinemethanol and a synthetic method thereof. According to the method, 2-picoline and hydrogen peroxide are taken as raw materials, glacial acetic acid is taken as a solvent, the mixture has a reaction for 3-5 hours at the temperature of 70 DEG C-80 DEG C under the action of a catalyst, and 2-picoline nitrogen oxide is obtained after separation; 2-picoline nitrogen oxide and acetic anhydride react for 3-6 hours under the reflux condition, and acetic acid-2 pyridine methyl ester is obtained after separation; acetic acid-2 pyridine methyl ester is directly hydrolyzed under the alkali separating condition by sodium hydroxide, and a product 2-pyridinemethanol is obtained after separation. 2-pyridinemethanol and the synthetic method have the benefits as follows: the selectivity of process target products is high, material loss is low, the product content and the total yield can reach 98.5% and 65% respectively, and 2-pyridinemethanol is suitable for industrial mass production.

Description

technical field [0001] The invention belongs to the technical fields of fine chemical production and pesticides, and in particular relates to a synthesis method of 2-pyridinemethanol and a product obtained by the method. Background technique [0002] 2-Pyridinemethanol, also known as 2-hydroxymethylpyridine, molecular formula C 6 h 7 NO, molecular weight 109.12, appearance is light yellow clear liquid, soluble in water and organic solvents, easily soluble in chloroform and methylene chloride, mainly used in pharmaceutical intermediates, non-steroidal anti-inflammatory drugs pyridinemethanol ibuprofen axetil, laxatives Bisacodyl and an intermediate of important drugs such as a newly developed drug for treating cardiovascular diseases have great potential for development. [0003] At present, there are relatively few literature reports on the research and development of 2-pyridinemethanol in my country, and most of them refer to foreign mature technologies for research and p...

Claims

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Application Information

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IPC IPC(8): C07D213/64
CPCY02P20/584C07D213/64
Inventor 袁晓路张涛赵广福葛德强赵志华黄成周寿芳周浩吴德清王晓亭
Owner ANHUI COSTAR BIOCHEM CO LTD
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