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Method for catalytic synthesis of 2-amino-5-chloropyridine by microwave synergistic lewis acidic ionic liquid

A technology of acidic ionic liquid and ionic liquid, which is applied in the direction of organic chemistry, can solve the problems of difficult separation of products, high cost, harsh reaction conditions, etc., and achieve the effects of shortening reaction time, low production cost and simplified production process

Inactive Publication Date: 2020-10-02
SHANDONG JINCHENG KERUI CHEMICAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] The purpose of the present invention is to overcome the deficiencies of the prior art and provide a method for synthesizing 2-amino-5-chloropyridine with microwave synergistic ionic liquid catalysis, aiming to solve the problems of high cost, harsh reaction conditions and difficult separation of products And other issues

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Under 50W microwave radiation, add 20g (0.21mol) 2-aminopyridine and 200mL acetone to a 500mL three-necked round-bottomed flask, stir and dissolve, then add 3.4g N-butylpyridinium chloride-aluminum trichloride ionic liquid, Then, 16 g (4.3 L) of chlorine gas was introduced, reacted for 45 min, recrystallized with methanol, and dried to obtain 24.6 g of 2-amino-5-chloropyridine-like white crystals with a GC purity of 99.6% and a molar yield of 90.0%.

Embodiment 2

[0025] Under 60W microwave radiation, add 20g (0.21mol) 2-aminopyridine and 200mL acetonitrile to a 500mL three-necked round-bottom flask successively, stir and dissolve, add 1.8g N-ethylpyridinium chloride-aluminum trichloride ionic liquid, Introduce 30g (9.46L) of chlorine gas, react for 50min, recrystallize with methanol, and dry to obtain 25.7g of 2-amino-5-chloropyridine-like white crystals with a GC purity of 99.4% and a molar yield of 99.4%.

Embodiment 3

[0027] Under the irradiation of a 160W blue LED lamp, add 20g (0.21mol) 2-aminopyridine and 200mL dichloromethane to a 500mL three-necked round-bottom flask in turn, stir and dissolve, then add 1.8g N-ethylpyridinium chloride-zinc chloride ion Liquid, after the solution fades, then 20g (6.3L) of chlorine gas is passed through, reacted for 30min, recrystallized by ethanol, and dried to obtain 26.1g of 2-amino-5-chloropyridine-like white crystals with a GC purity of 99.6% and a molar yield of 95.6%.

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Abstract

The invention relates to a method for catalytic synthesis of 2-amino-5-chloropyridine by microwave synergistic lewis acidic ionic liquid, which comprises the following steps: adding 2-aminopyridine asa raw material into an organic solvent, introducing chlorine under the action of a catalyst lewis acidic ionic liquid and microwave radiation, and carrying out chlorination reaction; and carrying outreduced pressure distillation on the obtained reaction solution to remove the solvent, and further recrystallizing the solution to obtain the high-purity 2-amino-5-chloropyridine. Compared with the prior art, the method has the advantages that the production process is simplified, the reaction conditions are mild, the product purity is higher, the lewis acidic ionic liquid can be recycled, and the production cost is low.

Description

technical field [0001] The invention belongs to the technical field of synthesizing 2-amino-5-chloropyridine, and in particular relates to a method for synthesizing 2-amino-5-chloropyridine under the catalysis of microwave and Lewis acidic ionic liquid. Background technique [0002] 2-Amino-5-chloropyridine is an important chemical intermediate widely used in the fields of medicine, pesticides and dyes. Many kinds of substances can be synthesized by using 2-amino-5-chloropyridine, such as sedative and hypnotic drug zopiclone, new anticoagulant drug edoxaban, etc. Parasite drugs. At present, domestic and foreign markets are in great demand, but there are not many reports on its synthesis in China. [0003] The synthetic method about this compound mainly takes 2-aminopyridine as raw material, and following several synthetic routes are arranged: [0004] (1) Thomas et al. proposed in their patent US3985759 that 2-aminopyridine was dissolved in a strong acid solvent, and chlo...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D213/73
CPCC07D213/73
Inventor 宋君房正薇崔宝龙于复刚陈钊
Owner SHANDONG JINCHENG KERUI CHEMICAL CO LTD
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