Method for synthesizing thiotriazinone

A synthesis method and technology of triazine ring, applied in the field of synthesis of pharmaceutical intermediates, can solve the problems of long overall reaction time, waste of time and raw materials, low reaction yield and the like, so as to shorten the reaction time, reduce the cost of raw materials, and reduce the operation effect of steps
CN102558080AActive Publication Date: 2012-07-11YIYUAN XINQUAN CHEM
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Patent Information

Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
YIYUAN XINQUAN CHEM
Publication Date
2012-07-11

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Abstract

The invention relates to a method for synthesizing a pharmaceutical intermediate, in particular to a method for synthesizing thiotriazinone. The method comprises the following steps of: reacting 2-methylaminothiourea and diethyl oxalate which are taken as raw materials and ethanol which is taken as a solvent to obtain crude thiotriazinone, and recrystallizing the crude thiotriazinone to obtain a final product, wherein a recrystallization solvent is water. The method is characterized in that: a catalyst is added in the reaction of the 2-methylaminothiourea and the diethyl oxalate, and is a mixture of ammonium chloride and a hydrochloric acid solution at the concentration of 10 weight percent. The method has the advantages that: the reaction yield is improved and the reaction time is shortened by selecting the appropriate catalyst; the cost of raw materials is reduced; operation steps are reduced; and the method is more suitable for industrialized production.
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Description

technical field

[0001] The invention relates to a method for synthesizing a pharmaceutical intermediate, in particular to a method for synthesizing a triazine ring. Background technique

[0002] Triazine ring, chemical name: 2,5-dihydro-6-hydroxy-2-methyl-5-oxo-3-mercapto-1,2,4-triazine, molecular formula: C 4 h 5 N 3 o 2 S, the structural formula is as follows:

[0003]

[0004] Appearance: White or off-white crystalline powder, melting point ≥ 245°C.

[0005] Triazine ring is an important pharmaceutical intermediate, mainly used in the synthesis of ceftriaxone sodium.

[0006] The triazine ring reacts with 2-methylthiosemicarbazide and diethyl oxalate as raw materials to generate the target compound. The reaction formula is as follows:

[0007]

[0008] However, there are problems such as low reaction yield and long overall reaction time, resulting in waste of time and raw materials, which greatly restricts actual production. Contents of the invention [00...

Claims

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