Method for synthesizing triazine ring

A synthesis method and technology of triazine ring, applied in the field of synthesis of triazine ring, can solve the problems of high cost of raw materials, complicated operation, low yield and the like, and achieve the effects of low cost of raw materials, high yield, and reduction of three-waste pollution

Inactive Publication Date: 2010-05-05
NANTONG NABAIYUAN CHEM
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  • Summary
  • Abstract
  • Description
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Problems solved by technology

[0013] The existing triazine ring synthesis method is complicated to operate, has many wastes, low yield and high cost of raw materials

Method used

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  • Method for synthesizing triazine ring

Examples

Experimental program
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Effect test

Embodiment 1

[0028] ①Put 40g of methylhydrazine aqueous solution and 29g of ammonium thiocyanate into a 500ml reaction flask, heat to reflux, and control the reaction temperature at 85-90°C. After removing the water under negative pressure, add 180g of methanol to obtain aminomethylhydrazine methanol solution .

[0029] ②Add 50g dimethyl oxalate and 118g sodium methoxide to the reacted aminomethylhydrazine methanol solution, heat and reflux for 6 hours, control the reaction temperature at 65-75°C, and adjust the pH value to 6-7 with hydrochloric acid to remove excess sodium methoxide, filtered, and the filtrate (triazine ring sodium salt solution) was acid-absorbed with hydrochloric acid to adjust the pH value to 1-2, and filtered to obtain a crude triazine ring.

[0030] ③The crude triazine ring was added to hot water, stirred, cooled and crystallized, filtered, and dried to obtain 41 g of triazine ring with a yield of 70%.

Embodiment 2

[0032] ①Put 40g of methylhydrazine aqueous solution and 29g of ammonium thiocyanate into a 500ml reaction flask, heat to reflux, and control the reaction temperature at 95-100°C. After removing the water under negative pressure, add 200g of methanol to obtain aminomethylhydrazine methanol solution.

[0033] ②Add 52g dimethyl oxalate and 122g sodium methoxide to the reacted aminomethylhydrazine methanol solution, heat and reflux for 6 hours, control the reaction temperature at 65-75°C, adjust the pH value to 6-7 with hydrochloric acid after the reaction, and filter , the filtrate is then adjusted to a pH of 1 to 2 with hydrochloric acid, filtered, and the filter cake is the crude product of the triazine ring.

[0034] ③ Add the crude triazine ring to an appropriate amount of hot water, stir, cool and crystallize, filter, and dry to obtain 44 g of the triazine ring with a yield of 75%.

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Abstract

The invention discloses a method for synthesizing triazine ring, which is implemented by reacting aqueous methylhydrazine solution with ammonium sulfocyanate, and then preparing amino methyl sulfourea methanol solution by using methanol; performing cyclization reaction on amino methyl sulfourea methanol solution with dimethyl oxalate and sodium methylate, adjusting pH value with hydrochloric acid after finishing cyclization reaction, removing excessive sodium methylate, and filtering to prepare triazine ring sodium salt; aciding out the triazine ring sodium salt to obtain a crude triazine ring product; agitating the crude triazine ring product with hot water, washing, cooling, crystallizing, and drying to obtain a fine triazine ring product. The invention has high yield and low material cost, reduces labor intensity and pollution of waste gas, waste water and industrial residue.

Description

Technical field: [0001] The invention relates to a synthesis method of a triazine ring. Background technique: [0002] triazine ring [0003] English name: Thiotriazinone [0004] CAS NO: 58909-39-0 [0005] Molecular weight: 159.16 [0006] EC NO: 261-490-1 [0007] Molecular formula: C 4 h 5 N 3 o 2 S [0008] Product introduction: Physical and chemical properties: Melting point ≥ 245°C [0009] Uses: Used as intermediates of ceftriaxone sodium, ceftriaxone sodium and other drugs. [0010] Alias: 2,5-dihydro-6-hydroxy-2-methyl-5-oxo-3-mercapto-1,2,4-triazine; triazine acid [0011] Structural formula: [0012] [0013] The existing method for synthesizing triazine rings has complex operations, many wastes, low yield and high cost of raw materials. Invention content: [0014] The object of the present invention is to provide a kind of synthetic method of the triazine ring that yield is high, raw material cost is low, reduces three wastes pollution. [001...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D253/07
Inventor 陆松林许陈兵陆群山吴建树宋美瑛
Owner NANTONG NABAIYUAN CHEM
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