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Method used for purifying sulfadimoxine

A cycle-effective sulfonamide and condition technology, applied in the direction of organic chemistry, can solve the problems of multiple impurities and mixed, and achieve the effect of improving the purity and yield

Inactive Publication Date: 2014-07-09
CHANGSHU NANHU INDAL CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Although the above method can improve the purity of sulfonamide, it is still mixed with more impurities

Method used

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  • Method used for purifying sulfadimoxine
  • Method used for purifying sulfadimoxine
  • Method used for purifying sulfadimoxine

Examples

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Embodiment 1

[0028] This example provides a kind of method of purifying sulfamethoxazole, and specific feeding ratio is as shown in Table 1:

[0029] Table 1 Reaction raw materials and their feeding ratio

[0030] raw material name

Feeding amount (kg)

molecular weight

Remark

Sulfonamide crude product

full batch

310.33

Deionized water

2400

18

Calcium hydroxide

20

74.08

activated carbon

12.5

12

Glacial acetic acid

35

60

[0031] The specific operation process is as follows:

[0032] (a) Add deionized water and calcium hydroxide to the reaction vessel, heat to 80-85°C, then add the crude sulfonamide product with stirring, then adjust the pH to 9.5-10.5 to make the crude sulfonamide product completely dissolve;

[0033] (b) adding active carbon in the container, after stirring for 1 hour under the condition of 80~85 DEG C, it is filtered through a single sh...

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Abstract

The invention relates to a method used for purifying sulfadimoxine. The method comprises following steps: (a) deionized water and calcium hydrate are delivered into a reaction container, an obtained mixture is heated to 80 to 85 DEG C, a sulfadimoxine coarse product is added with stirring, and pH value is adjusted to 9.5 to 10.5 so as to realize complete dissolving; (b) active carbon is delivered into the reaction container, an obtained mixed material is stirred for 0.5 to 2h at a temperature of 80 to 85 DEG C, and a filtrate is obtained via filtration; and (c) gracial acetate acid solution is added dropwise into the filtrate at a temperature of 75 to 80 DEG C, and then an obtained material is cooled via ice-water bath, pH value is adjusted to 5.1 to 5.4, the material is allowed to stand, and is subjected to centrifugal dewatering after precipitation, and a filter residue is collected. According to the method, gracial acetate acid solution is added dropwise into the filtrate, the obtained material is allowed to stand for precipitation, and is cooled via ice-water bath, so that sulfadimoxine can be precipitated rapidly, influences caused by other impurities are avoided, and purity and yield of sulfadimoxine are increased.

Description

technical field [0001] The invention relates to a preparation method of sulfonamide, in particular to a method for purifying sulfonamide. 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 has gradually stabilized, specifically the following preparation steps: [0003] step 1): [0004] [0005] Step (2): [0006] [0007] Step (3): [0008] [0009] Step (4): [0010] [0011] Step (5): [0012] [0013] The Chinese invention patent with the authorized notification number CN102304095B discloses a method for purifying sulfonamide, wh...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D239/69
CPCC07D239/69
Inventor 邵香民
Owner CHANGSHU NANHU INDAL CHEM