Refining method of 3-amino-2-(1, 3-dimethylbutyl) thiophene

Abstract

The invention discloses a refining method of 3-amino-2-(1, 3-dimethylbutyl) thiophene, and relates to the technical field of refining of chemical products. The method comprises the following steps: dissolving a raw material 3-benzoylamino-2-(1, 3-benzyl butyl) thiophene in n-caprylic alcohol to form a raw material solution, adding the raw material solution into a reaction kettle, adding potassium hydroxide, heating to 150 DEG C, reacting for 10 hours, detecting that the reaction is complete, cooling to 30 DEG C or below, adding 1% of silica gel into the reaction solution, filtering through a precision filter, and drying to obtain the 3-benzoylamino-2-(1, 3-benzyl butyl) thiophene. And adding activated carbon for adsorption, then washing with water, concentrating and recovering n-caprylic alcohol, and rectifying residual liquid obtained by concentration to obtain the product 3-amino-2-(1, 3-dimethylbutyl) thiophene. The content of 3-amino-2-(1, 3-dimethylbutyl) thiophene is increased from 98% obtained in the prior art to more than or equal to 99.9%.

Description

Technical Field

[0001] The invention relates to the technical field of chemical product refining, in particular to a method for refining 3-amino-2-(1,3-dimethylbutyl)thiophene. Background Art

[0002] 3-Amino-2-(1,3-dimethylbutyl)thiophene is mainly used for organic synthesis and applied in the field of electronic chemicals. It is a positive and negative electrode additive for batteries. It can effectively improve the conductivity, stability and cycle performance of electronic batteries and improve the utilization rate of electrode materials. At the same time, it also has the characteristics of good dispersibility, thickening and thixotropy. When added to the electrolyte solution as an additive in lithium batteries, it can reduce the interfacial tension, thereby increasing the solubility of active substances; in addition, it also has the effect of promoting solvent decomposition. The 3-amino-2-(1,3-dimethylbutyl)thiophene prepared by the existing technology has a low content, more impurities and low purity. Summary of the invention

[0003] In order to solve the above problems, that is, to solve the problems raised by the above background technology, the present invention proposes a method for refining 3-amino-2-(1,3-dimethylbutyl)thiophene, and the specific technical scheme is as follows:

[0004] A method for refining 3-amino-2-(1,3-dimethylbutyl)thiophene comprises the following steps: dissolving a raw material 3-benzamido-2-(1,3-benzylbutyl)thiophene in n-octanol to form a raw material solution, adding the raw material solution into a reaction kettle, adding potassium hydroxide, heating to 150°C, reacting for 10 hours, detecting that the reaction is complete, cooling to below 30°C, adding 1% silica gel to the reaction solution, filtering through a precision filter, adding activated carbon for adsorption, then washing with water, concentrating to recover n-octanol, and distilling the concentrated residual liquid to obtain the product 3-amino-2-(1,3-dimethylbutyl)thiophene.

[0005] Specifically, the raw material 3-benzamido-2-(1,3-benzylbutyl)thiophene is dissolved in n-octanol at a mass ratio of 1:4.

[0006] Specifically, the amount of potassium hydroxide added is 1.1 times the molar amount of the raw material 3-benzamido-2-(1,3-benzylbutyl)thiophene.

[0007] Specifically, the silica gel is 300 mesh fine pore silica gel.

[0008] Specifically, in the method, the reaction is carried out under the protection of an inert gas.

[0009] Specifically, in the method, the reaction is carried out under nitrogen protection.

[0010] Specifically, the final 3-amino-2-(1,3-dimethylbutyl)thiophene content is ≥99.9%.

[0011] The beneficial technical effect of the present invention is that some impurities that are difficult to remove by distillation are removed by filtering through fine-porous silica gel and precision filters, so that the content of 3-amino-2-(1,3-dimethylbutyl)thiophene is increased from 98% obtained by the original technology to a content of ≥99.9%. BRIEF DESCRIPTION OF THE DRAWINGS

[0012] Figure 1 is the reaction chemical formula of the method of the present invention. DETAILED DESCRIPTION

[0013] The preferred embodiments of the present invention are described below with reference to the accompanying drawings. It should be understood by those skilled in the art that these embodiments are only used to explain the technical principles of the present invention and are not intended to limit the protection scope of the present invention.

[0014] A method for refining 3-amino-2-(1,3-dimethylbutyl)thiophene, the specific method is as follows:

[0015] The raw material 3-benzamido-2-(1,3-benzylbutyl)thiophene is dissolved in n-octanol at a mass ratio of 1:4 to form a raw material solution, and the raw material solution is added to the reactor, and potassium hydroxide is added, wherein the amount of potassium hydroxide added is 1.1 times the molar amount of the raw material 3-benzamido-2-(1,3-benzylbutyl)thiophene. The temperature is raised to 150°C, and after reacting for 10 hours, the reaction is detected to be complete, and the temperature is lowered to below 30°C, 1% 300 mesh fine pore silica gel is added to the reaction solution, filtered through a precision filter, and activated carbon is added for adsorption, and then washed and concentrated to recover n-octanol, and the concentrated residual liquid is distilled to obtain the product 3-amino-2-(1,3-dimethylbutyl)thiophene.

[0016] A batch of 3-amino-2-(1,3-dimethylbutyl)thiophene was prepared using the prior art. As a comparative example, three groups of 3-amino-2-(1,3-dimethylbutyl)thiophene were prepared using the method of the present invention, as Examples 1-3. The experimental data of the products obtained from the two are as follows:

[0017] Group Example 1 Example 2 Example 3 Comparative Example Product purity (%) 98.03 99.91 99.90 99.92

[0018] It can be seen from the above test data that the purity of the 3-amino-2-(1,3-dimethylbutyl)thiophene product prepared according to the method of the present invention is generally higher than that of the 3-amino-2-(1,3-dimethylbutyl)thiophene prepared by the prior art, and the purity of the final product can be stabilized at more than 99.9%.

[0019] Although the present invention has been described with reference to preferred embodiments, various modifications may be made thereto and parts thereof may be replaced by equivalents without departing from the scope of the present invention. In particular, the various technical features mentioned in the various embodiments may be combined in any manner as long as there is no structural conflict. The present invention is not limited to the specific embodiments disclosed herein, but includes all technical solutions falling within the scope of the claims.

[0020] In the description of the present invention, the terms "center", "upper", "lower", "left", "right", "vertical", "horizontal", "inner", "outer" and the like indicating directions or positional relationships are based on the directions or positional relationships shown in the drawings, which are only for the convenience of description, and do not indicate or imply that the device or element must have a specific orientation, be constructed and operated in a specific orientation, and therefore cannot be understood as limiting the present invention. In addition, the terms "first", "second", and "third" are used for descriptive purposes only, and cannot be understood as indicating or implying relative importance.

[0021] In addition, it should be noted that in the description of the present invention, unless otherwise clearly specified and limited, the terms "installed", "connected", and "connected" should be understood in a broad sense, for example, it can be a fixed connection, a detachable connection, or an integral connection; it can be a mechanical connection or an electrical connection; it can be a direct connection, or it can be indirectly connected through an intermediate medium, or it can be the internal communication of two components. For those skilled in the art, the specific meanings of the above terms in the present invention can be understood according to specific circumstances.

[0022] The term "comprise" or any other similar term is intended to cover a non-exclusive inclusion, such that a process, article, or apparatus / device that includes a list of elements includes not only those elements but also other elements not expressly listed, or elements inherent to such process, article, or apparatus / device.

[0023] So far, the technical solutions of the present invention have been described in conjunction with the preferred embodiments shown in the accompanying drawings. However, it is easy for those skilled in the art to understand that the protection scope of the present invention is obviously not limited to these specific embodiments. Without departing from the principle of the present invention, those skilled in the art can make equivalent changes or substitutions to the relevant technical features, and the technical solutions after these changes or substitutions will fall within the protection scope of the present invention.

Claims

1. A method for refining 3-amino-2-(1,3-dimethylbutyl)thiophene, characterized in that: The method comprises the following steps: dissolving a raw material 3-benzylamino-2-(1,3-benzylbutyl)thiophene in n-octanol to form a raw material solution, adding the raw material solution into a reaction kettle, adding potassium hydroxide, heating to 150° C., reacting for 10 hours, detecting that the reaction is complete, cooling to below 30° C., adding 1% silica gel to the reaction solution, filtering through a precision filter, adding activated carbon for adsorption, then washing with water, concentrating and recovering n-octanol, and distilling the concentrated residual liquid to obtain the product 3-amino-2-(1,3-dimethylbutyl)thiophene.

2. A method for refining 3-amino-2-(1,3-dimethylbutyl)thiophene according to claim 1, characterized in that: The raw material 3-benzamido-2-(1,3-benzylbutyl)thiophene was dissolved in n-octanol at a mass ratio of 1:

4.

3. A method for refining 3-amino-2-(1,3-dimethylbutyl)thiophene according to claim 1, characterized in that: The amount of potassium hydroxide added is 1.1 times the molar amount of the raw material 3-benzamido-2-(1,3-benzylbutyl)thiophene.

4. A method for refining 3-amino-2-(1,3-dimethylbutyl)thiophene according to claim 1, characterized in that: The silica gel is 300 mesh fine pore silica gel.

5. A method for refining 3-amino-2-(1,3-dimethylbutyl)thiophene according to claim 1, characterized in that: In the method, the reaction is carried out under the protection of an inert gas.

6. A method for refining 3-amino-2-(1,3-dimethylbutyl)thiophene according to claim 4, characterized in that: In the method, the reaction is carried out under nitrogen protection.

7. A method for refining 3-amino-2-(1,3-dimethylbutyl)thiophene according to claim 1, characterized in that: The final 3-amino-2-(1,3-dimethylbutyl)thiophene content is ≥99.9%.

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