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Synthetic method of 3,4-dibromo sulfolane

A technology of dibromosulfolane and a synthesis method, which is applied in the field of synthesizing 3,4-dibromosulfolane, can solve the problems of poor heat and mass transfer, difficulty in stirring, difficult industrialized production and the like, and achieves the effects of simple process and high purity

Inactive Publication Date: 2013-04-17
ZHANGJIAGANG GUOTAI HUARONG NEW CHEM MATERIALS CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] It has been reported abroad that the addition of sulfolene and bromine was used to synthesize 3,4-dibromosulfolane without a solvent, but this process reacts without a solvent, and there are many inconveniences in production, such as difficulty in stirring, Poor heat and mass transfer, complex post-processing procedures, etc., making normal industrial production difficult

Method used

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  • Synthetic method of 3,4-dibromo sulfolane

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] Example 1 Add 59g of sulfolene and 59g of carbon tetrachloride into a round-bottomed four-necked flask equipped with a dropping funnel, condenser, stirrer and thermometer, raise the temperature to 90°C under stirring, add 80g of bromine dropwise, drop for about 30 minutes After the reaction is completed, the crude product liquid of 3,4-dibromosulfolane is obtained, the crude product liquid is filtered, the obtained solid is washed with carbon tetrachloride for 2 to 3 times, and the washed solid is dried 137.1 g of a white solid was obtained, which was 3,4-dibromosulfolane, with a purity of 99.5%, a melting point of 141-142°C, and a yield of 98.6%.

Embodiment 2

[0016] Example 2 Add 59g of sulfolene and 100g of carbon tetrachloride into a round-bottomed four-necked flask equipped with a dropping funnel, condenser, stirrer and thermometer, raise the temperature to 90°C under stirring, add 160g of bromine dropwise, drop for about 50 minutes After the reaction is completed, the crude product liquid of 3,4-dibromosulfolane is obtained, the crude product liquid is filtered, the obtained solid is washed with carbon tetrachloride for 2 to 3 times, and the washed solid is dried 136.2 g of a white solid was obtained, which was 3,4-dibromosulfolane, with a purity of 99.4%, a melting point of 141-142°C, and a yield of 98%.

Embodiment 3

[0017] Example 3 Add 59g of sulfolene and 100g of benzene into a round-bottomed four-necked flask equipped with a dropping funnel, a condenser, a stirrer and a thermometer, raise the temperature to 75°C while stirring, add 80g of bromine dropwise, drop it in about 30 minutes, continue Reacted at 75°C for 3 hours. After the reaction, the crude product liquid of 3,4-dibromosulfolane was obtained. The crude product liquid was filtered, and the obtained solid was washed twice with benzene, and the washed solid was dried to obtain 136.6 g of white solid. The solid is 3,4-dibromosulfolane with a purity of 99.3%, a melting point of 141-142°C and a yield of 98.3%.

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Abstract

The invention discloses a synthetic method of 3,4-dibromo sulfolane. The synthetic method comprises the steps of: (1) adding sulfolene to a solvent to obtain a sulfolene solution, then adding bromine to the sulfolene solution, reacting at 50-100 DEG C, thus obtaining a mixed liquid containing 3,4-dibromo sulfolane after ending reaction; and (2) filtering the mixed liquid, washing the obtained solid with the same solvent at least twice, and drying the washed solid to obtain 3,4-dibromo sulfolane, wherein the solvent is one of chloroform, carbon tetrachloride, benzene, methylbenzene and dimethylbenzene. The synthetic method is simple in process and has no pollution to the environment; the purity of 3,4-dibromo sulfolane prepared by the synthetic method is high and over 99%; the yield of 3,4-dibromo sulfolane is above 98%; and the synthetic method is suitable for industrial volume production.

Description

technical field [0001] The invention relates to a method for synthesizing 3,4-dibromosulfolane. Background technique [0002] Sulfolane is a new multi-effect solvent with excellent performance developed in the past 20 years. In addition to being used as an aromatic hydrocarbon extraction solvent, it can also be used as a purifying agent for natural gas, synthetic raw material gas and refinery gas, and an organic reaction solvent. , Polymer spinning or casting solvent, also can be used as plasticizer, dispersant, stabilizer, etc. 3,4-Dibromosulfolane is a derivative of sulfolane. Besides being used as a solvent, it can also be used as a pesticide, insecticide and pharmaceutical intermediate. [0003] It has been reported abroad that the addition of sulfolene and bromine was used to synthesize 3,4-dibromosulfolane without a solvent, but this process reacts without a solvent, and there are many inconveniences in production, such as difficulty in stirring, Poor heat and mass ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D333/48
Inventor 徐晓强李建中钱晓兵闻立新王一明
Owner ZHANGJIAGANG GUOTAI HUARONG NEW CHEM MATERIALS CO LTD
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