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Crystallization method of N-acetoacetanilide type compounds

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

Active Publication Date: 2015-02-25
青岛海湾集团有限公司
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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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  • Crystallization method of N-acetoacetanilide type compounds
  • Crystallization method of N-acetoacetanilide type compounds

Examples

Experimental program
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Effect test

Embodiment 1

[0032] A kind of crystallization method of N-acetoacetanilide compound, reaction kettle is stainless steel reaction kettle, and its schematic diagram is as figure 1 As shown, the stainless steel reaction kettle 1 is provided with a cooling pipe, and the cooling pipe includes an outer half pipe 2 arranged outside the reaction kettle and an inner coil pipe 3 arranged inside the reaction kettle.

[0033] Gradient cooling of the material is carried out by passing the condensing medium through the cooling pipe of the reactor, including the following steps:

[0034] (1) After the diacetylation reaction of aniline and diacetyl ketone with ethanol as a solvent in the reactor, feed circulating water at 15°C into the cooling tube, and control the temperature of the material from 60°C to 40°C within 40 minutes ; Stirring speed 60 rpm;

[0035] (2) After the first stage of cooling is completed, turn off the circulating water at 15°C, feed the circulating water at 7°C into the cooling pip...

Embodiment 2

[0039] A kind of crystallization method of N-acetoacetanilide compound, reaction kettle is stainless steel reaction kettle, and its schematic diagram is as figure 1 As shown, the stainless steel reaction kettle 1 is provided with a cooling pipe, and the cooling pipe includes an outer half pipe 2 arranged outside the reaction kettle and an inner coil pipe 3 arranged inside the reaction kettle.

[0040] Gradient cooling of the material is carried out by passing the condensing medium through the cooling pipe of the reactor, including the following steps:

[0041] (1) After the diacetylation reaction of aniline and diacetyl ketone with ethanol as a solvent in the reactor, feed circulating water at 16°C into the cooling tube to control the temperature of the material from 60°C to 40°C within 60 minutes ; Stirring speed 60 rpm;

[0042] (2) After the first stage of cooling is completed, turn off the circulating water at 16°C, feed the circulating water at 6°C into the cooling pipe,...

Embodiment 3

[0046] A kind of crystallization method of N-acetoacetanilide compound, reaction kettle is stainless steel reaction kettle, and its schematic diagram is as figure 1 As shown, the stainless steel reaction kettle 1 is provided with a cooling pipe, and the cooling pipe includes an outer half pipe 2 arranged outside the reaction kettle and an inner coil pipe 3 arranged inside the reaction kettle.

[0047] Gradient cooling of the material is carried out by passing the condensing medium through the cooling pipe of the reactor, including the following steps:

[0048](1) After the diacetylation reaction of 2,4-dimethylaniline and diacetyl ketone with ethanol as a solvent in the reactor finishes, feed circulating water at 14°C in the cooling tube to make the material within 50 minutes, Cool down from 60°C to 30°C; stirring speed 60 rpm;

[0049] (2) After the first stage of cooling is completed, turn off the circulating water at 14°C, and feed the circulating water at 7°C into the coo...

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Abstract

The invention relates to the field of synthesis of N-acetoacetanilide type compounds, and in particular relates to a crystallization method of N-acetoacetanilide. According to the crystallization method, gradient cooling is performed on materials by introducing a condensation medium into a cooling tube of a reaction kettle. The crystallization method disclosed by the invention is short in crystallization time, simple in operation step, capable of achieving automation and standardization and capable of improving the yield and purity of products, the particle sizes of product crystals are uniform and consistent, the phenomenon of agglomeration is further reduced, and the agglomeration time is greatly prolonged.

Description

technical field [0001] The invention relates to the field of synthesis of N-acetylacetanilide compounds, in particular to a crystallization method of N-acetylacetanilide compounds. Background technique [0002] Acetoacetanilide compounds are prepared by the condensation reaction of diketene and aniline compounds, and their basic structural formula is: [0003] [0004] The preparation method of the acetoacetanilide compound is as follows: react aniline and diketene to generate acetoacetanilide, and then filter and dry 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 an emulsifier to stirred deionized water at 0-10°C for reaction, and then Under temperature control, diketene and aniline were added dropwise at the same...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C231/24C07C231/04C07C235/80B01D9/02
Inventor 逄栋徐学锋王敦君
Owner 青岛海湾集团有限公司
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