Synthesis and crystallization method of N-acetoacetanilide compound

A technology for acetoacetanilide and aniline compounds, which is applied in the field of synthesis and crystallization of N-acetoacetanilide compounds, can solve the problems of high solvent consumption, influence on application, reduced yield and the like, and achieves reduced caking phenomenon and prolonged crystallization. The effect of short block time and crystallization time

Active Publication Date: 2015-02-18
QINGDAO DOUBLE PEACH SPECIALTY CHEM GRP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] Because the acetoacetanilide compound is in powder form, it is easy to agglomerate after long-term storage, which affects its application
And the smaller the particle size of the crystal, the more difficult it is to collect, the washing will consume a lot of solvent, and the yield will decrease

Method used

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  • Synthesis and crystallization method of N-acetoacetanilide compound
  • Synthesis and crystallization method of N-acetoacetanilide compound

Examples

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Embodiment 1

[0036] A method for the synthesis and crystallization of N-acetoacetanilide compounds. The reactor is a stainless steel reactor. The schematic diagram is as follows figure 1 As shown, the stainless steel reactor 1 is provided with a cooling tube, and the cooling tube includes an outer half tube (2) arranged outside the reactor and an inner coil 3 arranged inside the reactor.

[0037] It includes the following steps:

[0038] (1) Under anaerobic conditions, mix anilines with ethanol, and then add diketene for diacetylation to obtain acetoacetanilide compounds; the mixing temperature is 30°C, and the acetylation reaction time is 2 hours; diacetylated The reaction temperature is 30°C; after the diacetyl reaction is completed, the temperature of the heat preservation treatment is 40°C, and the heat preservation time is 3 hours;

[0039] (2 After the heat preservation is over, pass 15°C circulating water into the cooling pipe, and control the material to cool from 60°C to 40°C within 40 ...

Embodiment 2

[0044] A method for the synthesis and crystallization of N-acetoacetanilide compounds. The reactor is a stainless steel reactor. The schematic diagram is as follows figure 1 As shown, the stainless steel reactor 1 is provided with a cooling tube, and the cooling tube includes an outer half tube (2) arranged outside the reactor and an inner coil 3 arranged inside the reactor.

[0045] It includes the following steps:

[0046] (1) Under anaerobic conditions, mix anilines with ethanol, and then add diketene for diacetylation to obtain acetoacetanilide compounds; the mixing temperature is 30°C, and the acetylation reaction time is 2 hours; diacetylated The reaction temperature is 30°C; after the diacetyl reaction is completed, the temperature of the heat preservation treatment is 40°C, and the heat preservation time is 3 hours;

[0047] (2) After the heat preservation is over, pass 16°C circulating water into the cooling tube, and control the material to cool from 60°C to 40°C within 60...

Embodiment 3

[0052] A method for crystallization of N-acetoacetanilide compounds. The reactor is a stainless steel reactor. The schematic diagram is as follows figure 1 As shown, the stainless steel reactor 1 is provided with a cooling tube, and the cooling tube includes an outer half tube 2 arranged outside the reactor and an inner coil 3 arranged inside the reactor.

[0053] It includes the following steps:

[0054] (1) Under anaerobic conditions, mix 2,4-dimethylaniline with ethanol, and then add diketene for diacetylation to obtain acetoacetanilide compounds; the mixing temperature is 30°C, and the acetylation reaction time is 2 Hours; the reaction temperature of diacetylation is 30°C; after the completion of the diacetyl reaction, the temperature of the heat preservation treatment is 40°C, and the heat preservation time is 3 hours;

[0055] (2) After the heat preservation is over, pass 14°C circulating water into the cooling pipe to cool the material from 60°C to 30°C within 50 minutes; the...

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Abstract

The invention relates to the field of synthesis of N-acetoacetanilide compound, in particular to a synthesis and crystallization method of the N-acetoacetanilide compound. The synthesis method is to cool the material by feeding a condensation medium to a cooling pipe of a reaction kettle in a gradient manner. The crystallization method disclosed by the invention is short in crystallization time, simple in operation steps, capable of implementing automation and standardization, and further capable of increasing the yield and the purity of the product; the particle sizes of the crystals of the product are uniform and consistent; the agglomeration phenomenon can be further reduced; the agglomeration time can be greatly prolonged.

Description

Technical field [0001] The invention relates to the field of synthesis of N-acetoacetanilide compounds, in particular to a method for the synthesis and crystallization of N-acetoacetanilide compounds. Background technique [0002] Acetoacetanilide compounds are prepared by condensation reaction of diketene and aniline compounds. The basic structural formula is: [0003] [0004] The preparation method of the acetoacetanilide compound is: reacting aniline with diketene to generate acetoacetanilide, then filtering and drying to obtain the finished product. The acylation of diketene has the advantages of simple process, high yield and good quality. [0005] Patent application 201310136556.9 discloses a method for preparing N-acetoacetanilide. The specific steps of the method include: adding N-acetoacetanilide seed crystals and emulsifier to stirred deionized water at 0-10°C for reaction, and then at a certain temperature Diketene and aniline were added dropwise at the same time under ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C235/80C07C231/04C07C231/24B01J19/18
Inventor 赵秀平夏清合王永康
Owner QINGDAO DOUBLE PEACH SPECIALTY CHEM GRP
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