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Synthetic method for 2,2'-bipyridine

A technology of bipyridine and cyanopyridine, applied in 2 fields, can solve the problems of complex processing process, many side reactions, and high production cost

Inactive Publication Date: 2017-07-28
张燕梅
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

They have many side reactions, complicated process and high production cost

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] Example 1: Preparation of 2,2'-bipyridine

[0015] (1) Preparation of cyclooctadienyl cobalt

[0016] In a 250ml three-necked flask, add 100ml of tetrahydrofuran and 8g of sodium amide, add 20g of cyclooctadiene dropwise under stirring, and the temperature will rise. After the dropwise addition is completed, the temperature will be raised and refluxed for 2 hours. After the reaction is completed, the temperature will be reduced to room temperature for use; In a 500ml three-necked flask, add 100ml anhydrous tetrahydrofuran and 24g anhydrous cobalt chloride, stir and raise the temperature, when the temperature rises to 50℃, slowly add the above prepared solution dropwise, after the dropwise addition is complete, reflux and react for 5h, after the reaction is complete , Recover tetrahydrofuran. When the flow of tetrahydrofuran decreases, recover tetrahydrofuran under reduced pressure. After the recovery is complete, add 50g of 2-cyanopyridine, reduce to room temperature, and se...

Embodiment 2

[0019] Example 2: Preparation of 2,2'-bipyridine

[0020] (1) Preparation of cyclooctadienyl cobalt

[0021] In a 250ml three-necked flask, add 100ml of tetrahydrofuran and 5g of sodium metal, add 20g of cyclooctadiene dropwise under stirring, and the temperature will rise. After the dropwise addition is completed, the temperature will be raised and refluxed for 3 hours. After the reaction is completed, the temperature will be reduced to room temperature for use; In a 500ml three-necked flask, add 100ml anhydrous tetrahydrofuran and 24g anhydrous cobalt chloride, stir and raise the temperature, when the temperature rises to 50℃, slowly add the above prepared solution dropwise, after the dropwise addition, reflux for 4h, after the reaction is complete , Recover tetrahydrofuran. When the flow of tetrahydrofuran decreases, recover tetrahydrofuran under reduced pressure. After the recovery is complete, add 50g of 2-cyanopyridine, reduce to normal temperature, and seal for later use.

[...

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PUM

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Abstract

The invention specifically relates to a synthetic method for 2,2'-bipyridine, belonging to the field of chemical industrial synthesis. The synthetic method comprises the following successive steps: (1) reacting cyclooctadiene with anhydrous cobalt chloride under the catalysis of sodium amide (or metallic sodium) so as to produce cyclooctadiene-cyclopentadienyl cobalt which is a catalyst with high activity; and (2) reacting 2-cyanopyridine with acetylene gas under the catalysis of cyclooctadiene-cyclopentadienyl cobalt so as to produce 2,2'-bipyridine.

Description

Technical field [0001] The invention belongs to the field of chemical synthesis, and specifically relates to a synthesis method of 2,2'-bipyridine. Background technique [0002] 2,2'-Bipyridine is one of the isomers of bipyridine. It is an important organic synthesis intermediate, mainly used in pharmaceutical intermediates, organic synthesis, etc. It is also a widely used chelating agent and paint additive. , It is widely used in dye production, pesticide production and perfume. [0003] 2,2'-Dipyridyl, molecular formula: C10H8N2, molecular weight: 156.2, CAS NO: 366-18-7, English name: 2,2'-Dipyridyl, white or light red crystalline powder in appearance. [0004] The methods currently used in China: ① Anhydrous pyridine and anhydrous ferric chloride are mixed and heated to produce 2,2'-bipyridine; ②2-chloropyridine is coupled to react under the catalyst to produce 2,2,-bipyridine . They have many side reactions, complex treatment processes and high production costs. The synthesi...

Claims

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Application Information

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IPC IPC(8): C07D213/22C07D213/127B01J31/22
CPCB01J31/2295C07D213/127C07D213/22
Inventor 不公告发明人
Owner 张燕梅