Chemical synthesis method of 4-amino-3,5,6-trichloropyridine-2-formic acid

A technology of tetraclopyridine and triclopyridine, which is applied in the field of synthesis of organic compound herbicides, can solve the problems of high product cost, low product yield, large amount of waste water, etc., and achieve high reaction yield, low product cost, The effect of reaction time reduction

Inactive Publication Date: 2007-03-07
LIER CHEM CO LTD
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Problems solved by technology

If the proportion of ammoniating agent is reduced, the yield of product will be greatly reduced
At the same time, the amount of waste water produced by this reaction is relatively large, and the product cost is relatively high.

Method used

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  • Chemical synthesis method of 4-amino-3,5,6-trichloropyridine-2-formic acid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] In a 1000ml pressure-resistant reactor, add 12.8g (0.3mol) of sodium hydroxide and 750ml water, stir and dissolve, then add 83.1g (0.32mol, 94.2%) of tetraclopyridine, then add 150g liquid ammonia (8.82mol ), under the condition that the temperature is 110-125°C and the reactor is airtight, stir and react for 2.0 hours, release excess ammonia gas after the reaction is completed, then add hydrochloric acid to acidify to pH 1-2, filter and dry to obtain 70.6g product , the yield was 91.3%.

Embodiment 2

[0022] In a 1000ml autoclave, add potassium hydroxide 13.8g (0.3mol) and 750ml water, stir and dissolve, then add 83.1g (0.32mol, 94.2%) of tetraclopyridine, then add 150g liquid ammonia (8.82mol) , under the condition that the temperature is 110-120°C and the reactor is closed, the reaction is stirred for 2.5 hours. After the reaction is completed, excess ammonia gas is released, and then hydrochloric acid is added to acidify to pH 1-2. After filtration and drying, 68.8g of the product is obtained. Yield 89%.

Embodiment 3

[0024] In a 1000ml autoclave, add 750ml of water, then add 83.1g of tetraclopyridine (0.32mol, 94.2%), and then add 320g of ammonium carbonate (3.3mol). Under the conditions, the reaction was stirred for 3.0 hours. After the reaction was completed, hydrochloric acid was added to acidify to pH 1-2, and 67.2 g of the product was obtained after filtration and drying, with a yield of 87%.

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Abstract

The invention discloses a synthesizing method of new-typed herbicide 4-amino-3, 5, 6-trichloropyridine-2-aminic acid, which is characterized by the following: adopting 3, 4, 5, 6-tetrachloropyridine formate or tetrachloropyridine formic acid as original raw material; ammonifying; acidifying; making the total receiving rate at 75-91%.

Description

technical field [0001] The invention relates to a method for synthesizing an organic compound herbicide, in particular to a method for chemically synthesizing 4-amino-3,5,6-trichloropyridine-2-carboxylic acid. Background technique [0002] 4-Amino-3,5,6-trichloropyridine-2-carboxylic acid is a new herbicide. The literature has reported the method of taking heptachloromethylpyridine (SU445662) and 3,4,5,6-tetrachloropyridinenitrile (US4666384, AU8344982) as raw material synthesis respectively, because these two kinds of raw materials have poor solubility in water, Therefore, a large amount of water needs to be added as a solvent during the synthesis process, and the reaction temperature and pressure are relatively high. At the same time, it is necessary to react under the action of a large proportion of ammoniating agent, and the ratio of some ammoniating agent to tetrachlorocyanopyridine It is necessary to reach 62.85 times to obtain a 75% ammoniation yield. If the proport...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D207/34
Inventor 黄世伟
Owner LIER CHEM CO LTD
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