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Method for preparing 2- acetylthiophene

A technology of acetylthiophene and thiophene, which is applied in the field of 2-acetylthiophene preparation, can solve the problems of high environmental protection pressure and large industrial sewage

Inactive Publication Date: 2017-06-27
山西恒强化工有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0015] However, due to the extensive use of acid-base and organic solvent solutions in these process routes, a large amount of industrial sewage is generated, and the pressure on environmental protection is relatively high.

Method used

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  • Method for preparing 2- acetylthiophene

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preparation example Construction

[0038] The present invention provides a kind of green 2-acetylthiophene preparation method on the one hand, described method comprises the following steps:

[0039] First add thiophene, acetic anhydride and catalyst into the reaction kettle, react at 70-80°C for 3-5 hours, and then directly rectify to obtain the product. The remaining bottoms of the reactor can be directly applied to the next batch of reactions, and the next batch of reactions does not need to add catalysts.

[0040] In a preferred example of the present invention, the preparation method of 2-acetylthiophene is obtained by reacting thiophene with acetic anhydride in a solvent-free or organic solvent. This reaction can be carried out without adding a solvent, and the reaction can be carried out with a halogenated hydrocarbon such as thiophene, acetic anhydride, acetic acid, methylene chloride, chloroform, 1,2-dichloroethane as a solvent, preferably without a solvent.

[0041] In a preferred example of the pres...

Embodiment 1

[0046] and see attached figure 1, Add thiophene (84kg, purity 99%, provided by Shanxi Hengqiang Chemical Co., Ltd.) and acetic anhydride (102kg,) into the reactor, then add 500g of phosphoric acid, heat to 70-80°C, and react for 2-3 hours. After GC detection, the reaction is completed, rectified, and the product is collected according to the boiling point of the fraction. A total of 118kg (94% yield) of 2-acetylthiophene was obtained.

[0047] After the distillation is completed, add thiophene (84kg, purity 99%, provided by Shanxi Hengqiang Chemical Co., Ltd.) and acetic anhydride (102kg) into the reactor, heat to 70-80°C, and react for 2-3 hours. After GC detection, the reaction is completed, rectified, and the product is collected according to the boiling point of the fraction. A total of 120kg (95% yield) of 2-acetylthiophene was obtained. GC: 99.95%.

Embodiment 2

[0049] Add thiophene (84kg, purity 99%, provided by Shanxi Hengqiang Chemical Co., Ltd.), acetic anhydride (102kg,) and acetic acid (100kg) into the reactor, then add 500g of phosphoric acid, heat to 70-80°C, and react for 2-3 hours . After GC detection, the reaction is completed, rectified, and the product is collected according to the boiling point of the fraction. A total of 119kg (95% yield) of 2-acetylthiophene was obtained.

[0050] After the distillation is completed, add thiophene (84kg, purity 99%, provided by Shanxi Hengqiang Chemical Co., Ltd.), acetic anhydride (102kg), and acetic acid (100kg) into the reactor, heat to 70-80°C, and react 2 -3 hours. After GC detection, the reaction is completed, rectified, and the product is collected according to the boiling point of the fraction. A total of 120kg (95% yield) of 2-acetylthiophene was obtained. GC: 99.95%.

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Abstract

Provided is a method for preparing 2-acetylthiophene. The prepariaton method comprises the steps of first adding thiophene, acetic anhydride and a catalyst in a reaction kettle to react, and then directly performining rectification to obtain the product, wherein remaining substrate of the reaction kettle is used for a next batch of reactions, and the catalyst no longer needs to be added in the next batch of reactions. According the method, recycling of the the catalyst is achieved in the reaction process, the method not only reduces production cost and simplifies production process, but also enables the whole production process to be free of waste discharge, and green production of 2-acetylthiophene is achieved.

Description

technical field [0001] The invention relates to a method for preparing 2-acetylthiophene, in particular to a green method for preparing 2-acetylthiophene by first adding thiophene, acetic anhydride and a catalyst into a reactor for reaction, and then directly rectifying to obtain a product. Background technique [0002] 2-Acetylthiophene is an important chemical raw material intermediate, which is widely used in biomedicine, pesticides, polymer materials and conductive materials. [0003] Medical field: It is the intermediate 2-thiopheneacetic acid for the synthesis of broad-spectrum antibacterial drugs cephalothin, cefotaxime and cefoxitin, non-steroidal anti-inflammatory analgesic drug tiaprofen acid and 2-acetyl thienazine with anti-tumor activity It is an important raw material for transition metal Cu2+ and Fe2+ complexes. [0004] Chemical field: it is an important chemical reagent; because its gas chromatographic peak is closer to the peak of the drug intermediate 3-t...

Claims

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Application Information

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IPC IPC(8): C07D333/22
CPCY02P20/584C07D333/22
Inventor 方东严曙明方正飞沈国兵刘烨卢建军
Owner 山西恒强化工有限公司
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