Preparation method of triazine ring

A triazine ring and ring closure reaction technology, which is applied in the field of pharmaceutical intermediates, can solve the problems of inconvenient post-processing, low yield, and high cost, and achieve the effects of easy recrystallization and purification, reduced production costs, and simplified operating processes

Inactive Publication Date: 2013-07-31
HEILONGJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0013] The purpose of the present invention is to solve the problems of many by-products, high cost, low yield, inconvenient post-processing and

Method used

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  • Preparation method of triazine ring
  • Preparation method of triazine ring
  • Preparation method of triazine ring

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Experimental program
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specific Embodiment approach 1

[0026] Specific embodiment one: the preparation method of a kind of triazine ring of this embodiment is carried out according to the following steps:

[0027] 1. Using 2-methylthiosemicarbazide and diethyl oxalate as raw materials, using Lewis acid catalysis, under nitrogen protection, heating and melting, and then performing cyclization reaction, after the cyclization reaction is completed, it is lowered to room temperature to obtain a triazine ring Crude;

[0028] 2. After mixing the crude triazine ring obtained in step 1 with water, heating to reflux, filtering, collecting filtrate, then crystallizing by cooling, filtering, collecting filter cake, drying to obtain triazine ring;

[0029] Wherein, the molar ratio of 2-methylthiosemicarbazide to diethyl oxalate and Lewis acid described in step 1 is 1:(1~1.2):(0.01~0.05); the temperature of cyclization reaction is 120℃~ 150℃, the cyclization reaction time is 2~6h;

[0030] The quality of the water described in the second ste...

specific Embodiment approach 2

[0031] Embodiment 2: The difference between this embodiment and Embodiment 1 is that the Lewis acid described in step 1 is aluminum chloride, ferric chloride, boron trifluoride, titanium tetrachloride or zinc chloride. Others are the same as the first embodiment.

specific Embodiment approach 3

[0032] Embodiment 3: The difference between this embodiment and Embodiment 1 or 2 is that the Lewis acid described in Step 1 is aluminum chloride. Others are the same as in the first or second embodiment.

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Abstract

The invention relates to a preparation method of a triazine ring. The invention solves the problems that conventional preparation method of the triazine ring has the defects of many byproducts, high cost, low yield, inconvenient aftertreatment and unsuitability for large-scale production. The triazine ring is prepared from 2-methyl thiosemicarbazide and diethyl oxalate serving as starting raw materials through direct cyclization of a Lewis acid catalyst without any solvent system under the protection of nitrogen. The preparation method has the advantages of cheap and readily available raw materials, high yield, low cost and environment friendliness, and is suitable for industrial amplification. The preparation method is applied in the technical field of preparation of organic intermediates.

Description

technical field [0001] The invention relates to a preparation method of a triazine ring, belongs to the technical field of organic intermediate preparation, and is used as an intermediate of medicines such as ceftriaxone sodium and ceftriaxone. Background technique [0002] Triazine ring is an important organic intermediate, which has a wide range of applications in polymer materials, dyes, pesticides, and pharmaceutical industries, and has very important development value. [0003] English name: Thiotrzinone [0004] CASNO: 58909-39-0 [0005] Molecular formula: C 4 H 5 N 3 O 2 S; [0006] At present, the preparation method of triazine ring mainly has the following two kinds: [0007] Method 1 (Lu Songlin, Xu Chenbing, Lu Qunshan. Synthesis method of triazine ring, CN200910223937.4, 2009-11-20): [0008] [0009] This route uses 2-methylthiosemicarbazide and diethyl oxalate as raw materials, methanol as solvent, and sodium methoxide as catalyst. During cyclizatio...

Claims

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Application Information

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IPC IPC(8): C07D253/075
Inventor 张华迟帅李杨陈世杰崔玉祥苑兰兰沈明辉王雪微
Owner HEILONGJIANG UNIV
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