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5-methoxyl-4,6-dichloropyrimidine preparing method capable of preventing temperature fluctuation phenomenon from occurring

A technology of sodium methoxypyrimidine and dichloropyrimidine, which is applied in the field of preparation of sulfonamide intermediates, and can solve problems such as cross temperature and unfavorable reaction temperature

Inactive Publication Date: 2014-08-27
CHANGSHU NANHU INDAL CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the above reaction is prone to sudden temperature series when adding 4,6-dihydroxy-5-methoxypyrimidine sodium, about ten to twenty minutes, which is not conducive to the control of reaction temperature

Method used

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  • 5-methoxyl-4,6-dichloropyrimidine preparing method capable of preventing temperature fluctuation phenomenon from occurring
  • 5-methoxyl-4,6-dichloropyrimidine preparing method capable of preventing temperature fluctuation phenomenon from occurring
  • 5-methoxyl-4,6-dichloropyrimidine preparing method capable of preventing temperature fluctuation phenomenon from occurring

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preparation example Construction

[0021] The preparation method of 5-methoxy-4,6-dichloropyrimidine which does not produce dust and cross-temperature phenomenon of the present invention comprises the following steps: (a) adding phosphorus oxychloride into the reaction vessel, and then adding dropwise therein containing 4, The organic solvent of 6-dihydroxy-5-methoxypyrimidine sodium is refluxed at 110-120°C for 2-6 hours to obtain a reaction mixture; (b) adding the reaction mixture to deionized water for hydrolysis, and standing Layering to form the first water layer and the first organic solvent layer; (c) adding lye to the first organic solvent layer to adjust the pH value to 6.5-7, and standing to form the second water layer and the second organic solvent layer again Two organic solvent layers; (d) take the second organic solvent layer and distill off the organic solvent therein. On the one hand, reflux reaction at 110-120°C for 2-6 hours, so that the reaction can fully proceed; 4,6-dihydroxy-5-methoxypyri...

Embodiment 1

[0025] This example provides a preparation method of 5-methoxy-4,6-dichloropyrimidine, and the specific feeding ratio is shown in Table 1:

[0026] Table 1 Reaction raw materials and their feeding ratio

[0027]

[0028] The specific operation process is as follows:

[0029] (a) Add 825kg of phosphorus oxychloride into the dry chlorination reaction pot, turn on the reflux and hydrogen chloride gas absorption device, heat the chlorination reaction pot to 70°C with steam, turn off the steam and naturally heat up to 80°C; no dripping containing 4,6-dihydroxy-5-methoxypyrimidine sodium trichlorethylene control feeding time is 0.5-1.5 hours, so that the internal temperature is controlled at 80-95 ° C; heating, reflux at 110-120 ° C for 4 hours;

[0030] (b) Add the reaction mixture formed above into deionized water for hydrolysis, control the temperature not to exceed 60°C, let stand to separate layers to form a water layer and a trichlorethylene layer, extract the water layer...

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Abstract

The invention relates to a 5-methoxyl-4,6-dichloropyrimidine preparing method capable of preventing a temperature fluctuation phenomenon from occurring. The preparing method comprises the following steps that: (a) phosphorus oxychloride is added into a reaction container, then, organic solvents containing 4,6-dyhydroxyl-5-methoxyl pyrimidine sodium are added into the reaction container in a dropwise manner, and a reflux reaction is carried out for 2 to 6 hours at 110 to 120 DEG C to obtain a reaction mixture; (b) the reaction mixture is added into deionized water to be hydrolyzed, still standing layering is carried out, and a first water layer and a first organic solvent layer are formed; (c) alkali liquor is added into the first organic solvent layer for regulating the pH value to 6.5 to 7, the still standing layering is carried out again, and a second water layer and a second organic solvent layer are formed; and (d) the second organic solvent layer is distilled for removing the contained organic solvents. The organic solvents containing the 4,6-dyhydroxyl-5-methoxyl pyrimidine sodium are added into the reaction container in a dropwise manner, so the 4,6-dyhydroxyl-5-methoxyl pyrimidine sodium is diluted by the organic solvents; the adding speed of the 4,6-dyhydroxyl-5-methoxyl pyrimidine sodium can be controlled; the temperature of the reaction system can also be controlled; and the temperature fluctuation phenomenon cannot occur.

Description

technical field [0001] The invention relates to a preparation method of a sulfonamide intermediate, in particular to a preparation method of 5-methoxy-4,6-dichloropyrimidine which does not generate dust and cross temperature phenomenon. Background technique [0002] Sulfonamide, whose chemical name is 4-(p-aminobenzenesulfonyl)-5,6-dimethoxypyrimidine, is generally used for the treatment of inflammation, such as upper respiratory tract infection tonsillitis, bacillary enteritis, skin infection, etc. It can be used in conjunction with other drugs to treat pulmonary tuberculosis and lymphatic tuberculosis. Sulfonamide has gone through several generations of research and development, and its production process is gradually stable, specifically the following preparation steps: [0003] [0004] [0005] Wherein, 5-methoxy-4,6-dichloropyrimidine is an intermediate prepared in step (3), and its yield directly affects the yield and cost of sulfonamide. The Chinese invention...

Claims

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Application Information

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IPC IPC(8): C07D239/34
CPCC07D239/34
Inventor 邵香民
Owner CHANGSHU NANHU INDAL CHEM
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