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Preparation method of 3-carboxyl-4-hydroxy-acetoacetanilide

A technology of acetoacetanilide and hydroxyl, which is applied in the field of preparation of acetoacetanilide compounds, can solve the problems of low melting point and unfavorable application of acetoacetanilide compounds, and achieve the effects of simple operation steps, not easy to agglomerate, and mild reaction conditions

Inactive Publication Date: 2016-03-30
JIANGSU YANGTZE RIVER TIANYUE NEW MATERIALS
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  • Description
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AI Technical Summary

Problems solved by technology

Although the acetoacetanilide compound prepared by this method is not easy to agglomerate, the melting point of this acetoacetanilide compound is relatively low, which is unfavorable for the application of the acetoacetanilide compound

Method used

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  • Preparation method of 3-carboxyl-4-hydroxy-acetoacetanilide
  • Preparation method of 3-carboxyl-4-hydroxy-acetoacetanilide

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Embodiment Construction

[0020] The technical solution will be described in detail below in conjunction with specific embodiments, but the protection scope of the present invention is not limited to the embodiments.

[0021] A kind of preparation method of 3-carboxy-4-hydroxy-acetoacetanilide, the reaction equation of described preparation method is as follows:

[0022]

[0023] It is characterized in that: the preparation method comprises the following steps:

[0024] A. Pump the specified amount of soft water into the reaction kettle, then add caustic soda in the reaction kettle, start stirring until completely dissolved, and obtain sodium hydroxide solution;

[0025] B. Add 5-aminosalicylic acid to C 7 h 7 NO 3 Slowly add in the sodium hydroxide solution obtained in step A, stir until it is completely dissolved, adjust and measure the pH of the obtained mixed solution to ≈7;

[0026] C. Adjust the temperature in the reactor within the range of 18-27°C, slowly add diketene C 4 h 4 o 2 , th...

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Abstract

The invention discloses a preparation method of 3-carboxyl-4-hydroxy-acetoacetanilide. The preparation method comprises the following steps: pumping a prescribed amount of soft water into a reaction kettle, adding caustic soda flakes to the reaction kettle, slowly adding 5-aminosalicylic acid to a sodium hydroxide solution, and adjusting and determining the pH value of the above obtained mixed solution to be about 7; and adjusting the temperature in the reaction kettle to be 18-27DEG C, slowly adding diketene in a dropwise manner, carrying out heat insulation by using the natural temperature, discharging the obtained material to a neutralization and crystallization kettle, filtering, carrying out centrifuge dewatering, and drying to obtain a finished product. The method has the advantages of simple operating steps, good working environment, mild reaction conditions, no special requirements on a device, realization of good quality and high yield of the product, and low energy consumption, and the 3-carboxyl-4-hydroxy-acetoacetanilide prepared through the method is not likely to agglomerate.

Description

technical field [0001] The invention relates to a preparation method of acetoacetanilide compound, in particular to a preparation method of 3-carboxy-4-hydroxy-acetoacetanilide. Background technique [0002] Acetoacetanilide is a white crystalline powder, slightly soluble in water and easily soluble in organic solvents such as ethanol, ether, and chloroform. Acetoacetanilide can be used as an intermediate for organic pigments, dyes, and pesticides, and can be used to manufacture pyrazolone, bright yellow 5G, acid complex yellow GR, neutral deep yellow GL, neutral orange RL, sweat sand yellow G, pigment resistant Tanhuang G and the pesticide wilting, etc. 3-Carboxyl-4-hydroxyacetoacetanilide is a white powder crystal, CAS: 13243-99-7, mainly used in organic pigments, this product is an intermediate of dyes, organic pigments, and pesticides, and is used in the synthesis of neutral yellow dyes. Sexually integrated its GR, the production of organic yellow pigments. It is also...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C235/80C07C231/04
Inventor 陈睿沈永嘉丁秀萍陈阿明
Owner JIANGSU YANGTZE RIVER TIANYUE NEW MATERIALS
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