Preparation of 3-alkylthiophene

A technology of alkylthiophene and alkyl, which is applied in the field of preparation of 3-alkylthiophene, can solve problems such as unfavorable industrial production, limited source of raw materials, high reaction temperature, etc., achieve simple and easy operation process, easy control of reaction conditions, avoid the effect of

Inactive Publication Date: 2005-02-23
JIEXIN CHEM IND ZIBO CITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] The above four methods all require high reaction temperature and complex process equipment, and the source of raw materials is limited, which is not conducive to industrial production

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Add 15 ml of n-hexane and 0.1 g of ferric chloride into a 100 ml four-necked flask, stir vigorously, and cool to 0°C, add liquid A and liquid B evenly under stirring, liquid A is made of 10 ml of isoprene and 20 milliliters of n-hexane. Liquid B is a mixture of 4 milliliters of sulfur monochloride and 26 milliliters of n-hexane. During the dropwise addition, the reaction temperature was kept between -5 and 5°C, and the addition was completed in about 40 minutes. Then slowly rise to room temperature, and stir the reaction at room temperature for 3 days, distill off the n-hexane solvent, and transfer the residual liquid to a 50 ml distillation bottle, heat and reflux at 180-200°C for 5 hours, white acid mist is generated (lye neutralization treatment). After that, the temperature was lowered to below 60°C, and changed to a distillation device, heated to 120°C, and the distillate was collected. GC detection collected fractions with a purity above 99.0%, and obtained 0.83 ...

Embodiment 2

[0023] Add 15 ml of n-heptane and 0.1 g of ferric chloride into a 100 ml four-necked flask, stir vigorously, and cool to 0°C, add liquid A and liquid B evenly under stirring, liquid A is made of 10 ml of 2-ethane Base-1,3 butadiene and 20 ml of n-heptane, liquid B is a mixture of 4 ml of sulfur monochloride and 26 ml of n-heptane, keep the reaction temperature between -5 and 5°C during the dropwise addition , Add dropwise in about 40 minutes. Then slowly rise to room temperature, and stir the reaction at room temperature for 3 days, evaporate the n-heptane solvent, and transfer the residual liquid to a 50 ml distillation bottle, heat and reflux at 180-200 ° C for 5 hours, white acid mist Produced (lye neutralization treatment). After that, the temperature was lowered to below 60°C, and changed to a distillation device, heated to 120°C, and the distillate was collected. GC detection collected fractions with a purity above 99.0%, and obtained 0.92 g of pure 3-ethylthiophene wi...

Embodiment 3

[0025] Add 18 ml of low-boiling gasoline (60°C) and 0.12 g of ferric chloride into a 100 ml four-necked bottle, stir vigorously, and cool to 0°C, and drop liquid A and liquid B evenly under stirring, liquid A is made of 10 One milliliter of isoprene and 20 milliliters of low-boiling gasoline (60° C.), liquid B is a mixture of 4 milliliters of sulfur monochloride and 26 milliliters of low-boiling gasoline (60° C.), and the reaction temperature is kept at -5 during the dropwise addition. Between ~5°C, the dropwise addition is completed in about 40 minutes. Slowly rise to room temperature thereafter, and stir and react at room temperature for 3 days, distill off the low-boiling point gasoline (60°C) solvent, and move the residue to a 50-milliliter distillation bottle, heat and reflux at 180-200°C for 5 hours, White acid mist is produced (lye neutralization treatment). After that, the temperature was lowered to below 60°C, and changed to a distillation device, heated to 120°C, an...

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Abstract

A process for preparing 3-alkylthiophenium includes such steps as addition reaction between 2-alkyl-1,3-butadiene and sulfur monochloride under action of catalyst, and high-temp condensation-ring forming reaction.

Description

technical field [0001] The present invention relates to the preparation method of 3-alkylthiophene. Background technique [0002] 3-Alkylthiophene, mainly 3-methylthiophene and 3-ethylthiophene, are important intermediates such as medicines and pigments, and their synthesis methods have been reported in foreign literature, mainly as the following four more feasible processes route: [0003] One is that sodium methyl succinate and phosphorus sulfide are synthesized into 3-methylthiophene in the next step of carbon dioxide gas flow, and further refined to obtain a product with a yield of about 60% or more; [0004] The second is gas phase synthesis of 3-methylbutanol and carbon disulfide; [0005] The third is to add isoprene to high-temperature liquid sulfur to synthesize; [0006] The fourth is the synthesis of 2-methyl-2-butene and sulfur dioxide under the catalysis of metal salts. [0007] The above four methods all require high reaction t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D333/08
Inventor 戚聿新王庆鑫
Owner JIEXIN CHEM IND ZIBO CITY
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