Preparation method of besilate compound

A technology of benzenesulfonate and compounds, applied in the field of organic synthesis, can solve the problems of increasing operation complexity and high requirements of equipment, avoiding the use of sealing equipment and protective tools, facilitating operation and control, product yield and The effect of high purity

Active Publication Date: 2013-07-24
心邀(深圳)生物科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] S-(4- Tolyl)benzenesulfonate [see Journal of sulfur Chemistry, 2004, 25(5), p. 347-350], but this method uses thiophenol with foul smell and toxicity, so in the reaction process Closed operation is required, which increases the complexity of the operation and the high requirements of the equipment

Method used

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  • Preparation method of besilate compound
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  • Preparation method of besilate compound

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Embodiment 1: the synthesis of S-p-tolylbenzenesulfonate

[0030]

[0031] In terms of molar ratio, the ratio of benzenesulfonic acid, p-bromotoluene, sodium sulfide and oxidant is 1:1:1:0.5. Wherein oxidizing agent is hydrogen peroxide, and its mass percent concentration is 30%, and used solvent is benzene, and its quality is 5 times of benzenesulfonic acid quality, and concrete reaction process is as follows:

[0032] Slowly add benzenesulfonic acid into the solvent, stir evenly, then add p-bromotoluene dropwise, keep stirring during the dropwise addition, after the dropwise addition, continue stirring for 5-10 minutes to make the two evenly mixed, and then Add sodium sulfide and hydrogen peroxide respectively from two different feeding ports under continuous stirring, and after all the addition is completed, keep the reaction at this temperature for 1 hour. After the reaction was completed, saturated brine was added, and the organic layer was fully extracted. T...

Embodiment 2

[0034] Embodiment 2: the synthesis of S-p-tolylbenzenesulfonate

[0035] In terms of molar ratio, the ratio of benzenesulfonic acid, p-iodotoluene, sodium sulfide and oxidant is 1:2:2:1. Wherein oxidant is sodium hypochlorite, and used solvent is tetrahydrofuran, and its quality is 10 times of benzenesulfonic acid quality, and concrete reaction process is as follows:

[0036]Slowly add benzenesulfonic acid into the solvent, stir evenly, then add p-iodotoluene dropwise, keep stirring during the dropwise addition, after the dropwise addition, continue stirring for 5-10 minutes to make the two evenly mixed, and then Add sodium sulfide and sodium hypochlorite respectively from two different feeding ports under continuous stirring, and after all the addition is completed, keep the temperature for 2 hours for reaction. After the reaction was completed, saturated brine was added, and the organic layer was fully extracted. The organic layer was dried with anhydrous magnesium sulfat...

Embodiment 3

[0037] Embodiment 3: the synthesis of S-p-tolylbenzenesulfonate

[0038] In terms of molar ratio, the ratio of benzenesulfonic acid, p-chlorotoluene, sodium sulfide and oxidant is 1:3:3:1.5. Wherein oxidant is ammonium persulfate, and used solvent is ethanol, and its quality is 15 times of benzenesulfonic acid quality, and concrete reaction process is as follows:

[0039] Slowly add benzenesulfonic acid into the solvent, stir evenly, then add p-chlorotoluene dropwise, keep stirring during the dropwise addition, after the dropwise addition, continue stirring for 5-10 minutes to make the two evenly mixed, and then Add sodium sulfide and ammonium persulfate respectively from two different feeding ports under continuous stirring, and after all the addition is completed, keep the temperature for 3 hours for reaction. After the reaction was completed, saturated brine was added, and the organic layer was fully extracted. The organic layer was dried with anhydrous magnesium sulfate...

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Abstract

The invention relates to a preparation method of a besilate compound. The preparation method of the besilate compound comprises the following steps of: enabling benzenesulfonic acid, halobenzene and sodium sulphide to react in the presence of a solvent and an oxidant to obtain a target product containing besilate. The preparation method of the besilate compound is simple to operate, cheap in materials, high in product yield, high in purity and good in industrial application prospect.

Description

technical field [0001] The invention relates to a preparation method of an ester compound, in particular to a preparation method of a benzenesulfonate ester compound, and belongs to the field of organic synthesis. Background technique [0002] In the field of organic chemistry, benzenesulfonate compound is an important pharmaceutical intermediate and chemical intermediate, which can be used to carry out a variety of organic reactions to introduce different active groups or introduce benzenesulfonate into the final target product Groups, etc., for example, can be used as benzene sulfide reagents in organic reactions. [0003] Especially in the field of pharmaceutical compounds, compounds containing benzenesulfonate groups usually have a variety of biological activities and can be used for the synthesis of various drug intermediates. [0004] Just because of its wide application and importance, people have carried out a lot of in-depth research on the synthesis of benzenesulf...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C381/04
Inventor 竺叶洪
Owner 心邀(深圳)生物科技有限公司
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