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Preparation method of 1-chloro-6-iodohexane

A technology of iodohexane and chlorohexyl ester, which is applied in the field of preparation of 1-chloro-6-iodohexane, can solve the problems of difficult operation and high cost, achieve easy control of the production process, reduce the difficulty of reaction, and reduce the difficulty of operation Effect

Inactive Publication Date: 2019-03-19
三门峡奥科化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The present invention aims to provide an improved preparation method of 1-chloro-6-iodohexane, so as to overcome the existing technical defects such as high cost and difficult operation, and realize industrial scale production of 1-chloro-6-iodohexane

Method used

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  • Preparation method of 1-chloro-6-iodohexane

Examples

Experimental program
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Effect test

Embodiment 1

[0015] Synthesis of 4-methylbenzenesulfonic acid-6-chlorohexyl ester

[0016] Add 50mL sodium hydroxide aqueous solution (the sodium hydroxide is 4mol / L), 0.5gTEBA and 10.0g 6-chloro-1-hexanol into the reaction kettle, cool in ice / water bath, and slowly add 15.0g p-toluene dropwise under rapid stirring 50mL benzene solution of sulfonyl chloride, the reaction temperature is controlled at -5~0°C, the dropwise addition is completed in 2 hours, and the reaction is continued for 2 hours, left to stand, separated, dried, and benzene is recovered by atmospheric distillation to obtain 21.3g of 4-methylbenzenesulfonate Acid-6-chlorohexyl crude product (content 90%).

[0017] Synthesis of 1-chloro-6-iodohexane

[0018] Add the above crude product and 10.88g of sodium iodide into 50mL of acetone, stir vigorously, reflux for 1 hour, cool, stand, filter, and the filtrate is distilled under normal pressure to recover acetone, then rectified, and the fraction at 82°C is collected as product...

Embodiment 2

[0020] Synthesis of 4-methylbenzenesulfonic acid-6-chlorohexyl ester

[0021] Add 50mL sodium hydroxide aqueous solution (the sodium hydroxide is 4mol / L), 0.6gTEBA and 10.0g 6-chloro-1-hexanol into the reaction kettle, cool in ice / water bath, and slowly add 16.5g p-toluene dropwise under rapid stirring 50mL toluene solution of sulfonyl chloride, the reaction temperature is controlled at 0~5°C, the dropwise addition is completed in 2 hours, and the reaction is continued for 2 hours, left to stand, separated, dried, and the toluene is recovered by atmospheric distillation to obtain 21.6g of 4-methylbenzenesulfonic acid -Crude 6-chlorohexyl ester (content 91%).

[0022] Synthesis of 1-chloro-6-iodohexane

[0023] Add the above crude product and 11.97g of sodium iodide to 50mL of acetone, stir vigorously, reflux for 1 hour, cool, let stand, filter, the filtrate is distilled under normal pressure to recover acetone, and then rectified, and the fraction at 82°C is collected as prod...

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Abstract

The invention discloses a preparation method of 1-chloro-6-iodohexane. The preparation method comprises the steps of with 6-chloro-1-hexanol and p-toluene sulfochloride as the materials and benzene ortoluene as a solvent, reacting at (-5)-(5) DEG C for 2-5 hours under the effects of a phase transfer catalyst and an acid-binding agent so as to prepare 4-methylbenzenesulfonic acid-6-chlorohexyl ester, and carrying out reflux reaction on 4-methylbenzenesulfonic acid-6-chlorohexyl ester and sodium iodide for 0.5-3 hours, so as to prepare 1-chloro-6-iodohexane. The preparation method has the characteristics of easiness in operation, simplicity and convenience in after-treatment and relatively high yield.

Description

technical field [0001] The invention belongs to the technical field of fine chemicals, and in particular relates to a preparation method of 1-chloro-6-iodohexane. Background technique [0002] 1-Chloro-6-iodohexane is a colorless or light yellow transparent liquid, and it is an important intermediate for the preparation of pesticides and medicines, so it has a good market prospect. [0003] The traditional method for preparing 1-chloro-6-iodohexane is to use acetone as a solvent, and 1,6-dichlorohexane and sodium iodide as raw materials to obtain through iodine exchange reaction (for example: Journal of the Chemical Society, 2100-3; 1950; Australian Journal of Chemistry, 32(12), 2777-81; 1979). This scheme is simple to operate, but the reaction time is long, the reaction is incomplete, and the obtained products are 1-chloro-6-iodohexane and 1,6-diiodohexane, which are difficult to separate, and only about 50% of them are obtained after rectification The 1-chloro-6-iodohexa...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C19/07C07C17/093C07C309/73C07C303/28
CPCC07C17/093C07C303/28C07C309/73C07C19/07
Inventor 赵松芳杨凡刘之华尚晓冬姜守相郭超霞袁淑芳
Owner 三门峡奥科化工有限公司
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