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Synthetic method for 2,3-dipicolinic acid

A technology of dipicolinic acid and a synthesis method, which is applied in the field of synthesis of 2,3-pyridinedicarboxylic acid, can solve the problems of difficult catalyst recovery, complicated product separation, low product yield and the like, and achieves improved ring-opening oxidation effect, The effect of easy activation and increasing electron cloud density

Inactive Publication Date: 2018-12-14
XUZHOU NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The most important method of synthesizing 2,3-pyridinedicarboxylic acid is potassium permanganate oxidation quinoline method, which has difficulty in catalyst recovery, complicated product separation and low product yield

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] A kind of synthetic method of intermediate 2,3-pyridinedicarboxylic acid, the method comprises the following steps:

[0020] Step 1. Take 25g of CuSO 4 ·5H 2 O and 2mol L -1 110ml of sulfuric acid was added to a 500ml three-neck flask, stirred by magnetic force for 10min, and the CuSO 4 ·5H 2 After O is completely dissolved, 2g of catalyst Mn-TCPP and 13g of benzopyridine are added to the system and the temperature is raised;

[0021] Step 2. When the reaction temperature reached 100°C, 152 g of sodium chlorate aqueous solution with a concentration of 28% was added dropwise. After the dropwise addition, the reaction was kept for 6 hours, and a large amount of blue thick precipitate was formed;

[0022] Step 3, filter the reacted system while it is hot, wash the filter cake with hot water at 40°C until neutral, and dry for 3 hours to obtain the filter cake;

[0023] Step 4. Add the dried filter cake and 100g of 20% sodium hydroxide aqueous solution into a three-neck...

Embodiment 2

[0033] Step 1. Take 20g of CuSO 4 ·5H 2 O and 2mol L -1 110ml of sulfuric acid was added to a 500ml three-neck flask, stirred by magnetic force for 10min, and the CuSO 4 ·5H 2 After O was completely dissolved, 2g of catalyst Mn-TCPP and 13g of benzopyridine were added to the system and the temperature was raised; the rest of the steps were the same as in Example 1.

Embodiment 3

[0035] Step 1. Take 15g of CuSO 4 ·5H 2 O and 2mol L -1 110ml of sulfuric acid was added to a 500ml three-neck flask, stirred by magnetic force for 10min, and the CuSO 4 ·5H 2 After O was completely dissolved, 2g of catalyst Mn-TCPP and 13g of benzopyridine were added to the system and the temperature was raised; the rest of the steps were the same as in Example 1.

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Abstract

The invention discloses a synthetic method for 2,3-dipicolinic acid. According to the invention, CuSO4.5H2O, sulfuric acid, sodium quinoline chlorate, methyl 4-formylbenzoate, pyrrole, H2TCPP-OMe andMnCl2.6H2O are used as raw materials. The synthetic method of the invention uses quinoline for oxidative ring-opening in the oxidation system of NaClO3-H2SO4-CuSO4 under the action of the catalyst Mn-TCPP and then successively carries out alkali hydrolysis and acidification to obtain 2,3-dipicolinic acid. As the phenyl ring and the double bond of the catalyst Mn-TCPP are connected with electron-donating groups, electron cloud density on the double bond can be increased, and it is easier to attack and activate reactant intermediates; so ring-opening oxidation effect is improved, and yield is significantly higher than the yield of products obtained by conventional oxidation of potassium permanganate.

Description

technical field [0001] The invention relates to a method for synthesizing 2,3-pyridinedicarboxylic acid, which belongs to the field of chemical synthesis. Background technique [0002] 2,3-Pyridinedicarboxylic acid (2,3-Pyridinedicarboxylic acid) CAS: 89-00-9 is an intermediate in the synthesis of pesticides, medicines and dyes. It is widely used in many aspects such as drug synthesis and industrial synthesis. It can be used to synthesize p-fluorophenethyl ether, moxifloxacin, nicothamide, nicotinic acid, imidazolinone herbicides and quinolone antibiotics, etc. It is also a copper ion determination reagent. In addition, 2,3-pyridinedicarboxylic acid is a commonly used organic ligand in the synthesis of coordination polymers due to its stable properties. The most important method for synthesizing 2,3-pyridinedicarboxylic acid is potassium permanganate oxidation quinoline method, which has difficulty in catalyst recovery, complicated product separation and low product yield. ...

Claims

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Application Information

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IPC IPC(8): C07D213/79C07D213/807B01J31/32
CPCB01J31/32C07D213/79C07D213/807
Inventor 陈浩邵亚康建荣
Owner XUZHOU NORMAL UNIVERSITY
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