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Synthetic method of 2-amino-3,5-dibromopyridine

A dibromopyridine and synthesis method technology, applied in the field of synthesis of 2-amino-3,5-dibromopyridine, can solve the problems of many by-products, high price, cumbersome operation, etc., and achieve mild reaction conditions and stable product quality , post-processing simple effects

Inactive Publication Date: 2014-09-03
SHANDONG YOUBANG BIOCHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] (1) There are many by-products, resulting in a darker color of the product, which is difficult to refine and purify
Although it can be recrystallized multiple times with organic solvents, the quality still cannot meet the high requirements, and repeated crystallization leads to low product yield, increased cost, and cumbersome operation;
[0005] (2) The chemical reduction method used has serious corrosion of equipment and environmental pollution, and its development has been restricted at present;
[0006] (3) The source of raw materials is limited, the price is expensive, and the operation is troublesome;
[0007] (4) Need to use noble metal catalyst, increased preparation cost

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Add 2-amino-5-bromopyridine (3.46g, 20mmol), N-bromosuccinimide (7.12g, 40mmol) and methanol 15ml into a 50mL single-necked round bottom flask. The mixture in the reaction flask was stirred and reacted at 20°C for 4 hours. TLC and GC confirmed the completion of the reaction. After the reaction, the solvent was removed by rotary evaporation to obtain the crude product, which was separated by silica gel column chromatography to obtain the pure product 2-amino-3,5-dichloropyridine. After drying, the calculated yield was 67.06%, and the purity was 97.28% (GC). Melting point 102°C-105.2°C (98°C-106°C in literature).

Embodiment 2

[0020] Add 2-amino-5-bromopyridine (3.46g, 20mmol), N-bromosuccinimide (7.12g, 40mmol) and 18ml of ethanol into a 50mL single-necked round bottom flask. The mixture in the reaction flask was stirred and reacted at 20°C for 4 hours. TLC and GC confirmed the completion of the reaction. After the reaction, the solvent was removed by rotary evaporation to obtain the crude product, which was separated by silica gel column chromatography to obtain the pure product 2-amino-3,5-dichloropyridine. After drying, the calculated yield was 60.82%, and the purity was 98.05% (GC) , melting point 102°C-105.2°C (literature 98°C-106°C).

Embodiment 3

[0022] Add 2-amino-5-bromopyridine (17.30 g, 100 mmol), N-bromosuccinimide (40.94 g, 230 mmol) and 120 ml of ethyl acetate into a 500 mL single-necked round bottom flask. The mixture in the reaction flask was stirred and reacted at 20°C for 6 hours. TLC and GC confirmed the completion of the reaction. After the reaction, the solvent was removed by rotary evaporation to obtain the crude product, which was separated by silica gel column chromatography to obtain the pure product 2-amino-3,5-dichloropyridine. After drying, the calculated yield was 72.36%, and the purity was 97.28% (GC). Melting point 102°C-105.2°C (98°C-106°C in literature).

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Abstract

The invention belongs to the field of organic synthesis and in particular relates to a synthetic method of 2-amino-3,5-dibromopyridine. The synthetic method of 2-amino-3,5-dibromopyridine comprises the following steps: reacting raw materials including 2-amino-5-bromopyridine and N-chlorosuccinimide for 1-28 hours in a molar weight of 1:(0.5-5) in a proper solvent at 0-100 DEG C to generate a 2-amino-3,5-dibromopyridine crude product and purifying to obtain the pure product 2-amino-3,5-dibromopyridine. The synthetic method has the beneficial effects that the reaction raw materials are available and are reasonable in prices; the reaction conditions are mild; the synthetic method is easy to operate and control and is simple in aftertreatment; the product has stable quality and high purity.

Description

(1) Technical field [0001] The invention belongs to the field of organic synthesis, and in particular relates to a synthesis method of 2-amino-3,5-dibromopyridine. (2) Background technology [0002] 2-Amino-3,5-dibromopyridine is an important intermediate in organic synthesis, mainly used in pharmaceutical intermediates, organic synthesis, organic solvents, and can also be used in dye production, pesticide production and spices. [0003] The preparation of existing 2-amino-3,5-dibromopyridine has the following disadvantages: [0004] (1) There are many by-products, resulting in a darker color of the product, which is difficult to refine and purify. Although organic solvents can be used to recrystallize multiple times, the quality still cannot meet the high requirements, and repeated crystallization leads to low product yield, increased cost, and cumbersome operation; [0005] (2) The chemical reduction method used has serious corrosion of equipment and environmental pollut...

Claims

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Application Information

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IPC IPC(8): C07D213/73
CPCC07D213/73
Inventor 耿宣平来新胜曹惊涛
Owner SHANDONG YOUBANG BIOCHEM TECH
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