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Method for producing 2-pyridine formaldehyde

A technology of pyridine formaldehyde and its production method, which is applied in the direction of organic chemistry, can solve the problems of high energy consumption and heavy pollution, and achieve the effects of high product conversion rate, less reaction waste and low production cost

Inactive Publication Date: 2015-02-04
江苏常州酞青新材料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The purpose of the present invention is to solve the above-mentioned problems, provide a kind of improved production technology of 2-pyridine formaldehyde, so as to completely solve the high energy consumption in the original 2-pyridine formaldehyde production process, a kind of technical problems such as heavy pollution The production method of 2-pyridinecarbaldehyde

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Take 0.1mol of 2-picoline, a dichloromethane solution containing 0.1mol of 1M nitroglycerin, 55g of dichloromethane, and 9.5 mg of palladium chloride are mixed at room temperature, stirred for 3 hours, and 0.15mol of hydroxylamine hydrochloride is added to obtain about 10.6g of a white precipitate (86.9% yield).

Embodiment 2

[0026] Take 0.1mol of 2-picoline, a dichloromethane solution containing 0.1mol of 1M nitroglycerin, 20g of dichloromethane, and 27.1 mg of palladium chloride, mix at room temperature, stir for 3 hours, add 0.15mol of hydroxylamine hydrochloride, and obtain about 9.9g of white precipitate (81.1% yield).

Embodiment 3

[0028] Take 0.1mol of 2-picoline, dichloromethane solution containing 0.1mol 1M nitroglycerin, 9.3g of dichloromethane, 19 mg of palladium chloride, mix at room temperature, stir for 3 hours, add 0.15mol of hydroxylamine hydrochloride, and obtain a white precipitate of about 8.1 g (66.4% yield).

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Abstract

The invention discloses a method for producing 2-pyridine formaldehyde, wherein the method comprises the following steps: 2-methyl pyridine is subjected to a reaction for about 3 hours under a normal temperature condition and with use of a catalytic synthesis system, and thus 2-pyridine formaldehyde with the purity of more than 99.5% is obtained through oxime formation and a followed hydrolysis method. The method adopts a method of utilizing nitroglycerine to promote palladium chloride air oxidation, achieves green synthesis of pyridine formaldehyde under normal temperature and pressure conditions, has less reaction waste, is easy to process, low in production cost, and high in product conversion rate, achieves one step synthesis, and has better production convenience.

Description

technical field [0001] The invention relates to a production method of 2-pyridinecarbaldehyde. [0002] Background technique [0003] 2-Pyridinecarbaldehyde is a key intermediate of bisacodyl and other drugs. Its traditional synthesis techniques include 2-picoline chlorination to prepare 2-pyridinecarbaldehyde, and 2-pyridinemethanol oxidation. , production difficulty and other defects. Especially 2-picoline chlorination technology often needs to use more active chlorides such as thionyl chloride and 2-picoline chlorination to produce and process 2,2-dichloropicoline, so the production process is polluted The waste is higher and the production is more difficult. [0004] Contents of the invention [0005] The purpose of the present invention is to solve the above-mentioned problems, provide a kind of improved production technology of 2-pyridine formaldehyde, so as to completely solve the high energy consumption in the original 2-pyridine formaldehyde production process...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D213/48
CPCC07D213/48C07D213/53
Inventor 蒋明
Owner 江苏常州酞青新材料科技有限公司
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