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Beta-alkyl sulfide substituted vinyl propionate sulfur compound and preparation method thereof

A technology of vinyl acrylate and vinyl propionate, applied in the chemical field, can solve problems such as residual side reactions and harmful effects, and achieve the effects of wide application range, good yield, and practical industrial application value

Inactive Publication Date: 2012-11-21
HUAIYIN TEACHERS COLLEGE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Such addition reactions usually use strong bases and strong acids to activate nucleophiles or acceptors, which bring harmful residues and some side reactions to the environment

Method used

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  • Beta-alkyl sulfide substituted vinyl propionate sulfur compound and preparation method thereof
  • Beta-alkyl sulfide substituted vinyl propionate sulfur compound and preparation method thereof
  • Beta-alkyl sulfide substituted vinyl propionate sulfur compound and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0057] In a 200mL conical flask with ground mouth, first add 50mL of ionic liquid hydroxide [1-butyl-3-methylimidazole], then add 0.1mol thiophenol to the conical flask, mix well and then add 0.12mol formazan vinyl acrylate at 1kg / cm 2 Pressure, 20°C constant temperature shaking incubator, shake at a speed of 200 rev. / min; TLC monitors the reaction process, and it shows that the reaction is complete after 10 minutes, and the components of the reaction solution are detected by GC chromatography, such as image 3 ; image 3 middle t R =5.828 is the chromatographic peak of thiophenol, t R =7.169 is the chromatographic peak of the product; Add 60mL of ethyl acetate to the reaction solution to extract 5 times after the end, after the extracts are combined, the water pump decompression distillation reclaims ethyl acetate, the resulting product yield is 93%, and the infrared spectrum is characterized by Figure 4 , characterized by H NMR spectroscopy as Figure 5 , characterized ...

Embodiment 2

[0064] In a 200ml ground-mouth conical flask, first add 50ml of ionic liquid hydroxide [1-butyl-3-methylimidazole], then add 0.1mol thiophenol to the conical flask, mix well and add 0.12mol croton Acetate vinyl ester, at 1kg / cm 2 Pressure, 20°C constant temperature shaking incubator, shake at a speed of 200 rev. / min; TLC monitors the reaction process, and it shows that the reaction is complete after 10 minutes. After the end, add 60ml of ethyl acetate to the reaction solution for extraction 5 times, and the extracts are combined Afterwards, the water pump depressurized distillation to recover ethyl acetate, and the yield of the obtained product was 95%. See Figure 7 , see Figure 8 .

Embodiment 3

[0066]In a 50ml ground-mouth conical flask, first add 10ml of ionic liquid hydroxide [1-butyl-3-methylimidazole], then add 0.1mol benzyl mercaptan to the conical flask, mix thoroughly and add 0.12mol Vinyl methacrylate at 1kg / cm 2 Pressure, 25°C constant temperature shaking incubator, shake at a speed of 200 rev. / min; TLC monitors the reaction process, and it shows that the reaction is complete after 2 minutes. After the end, add 60ml of ethyl acetate to the reaction solution for extraction 5 times, and the extracts are combined Afterwards, the water pump depressurized distillation to recover ethyl acetate, and the yield of the obtained product was 91%. See Figure 9 , see Figure 10 .

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Abstract

The invention discloses a beta-alkyl sulfide substituted vinyl propionate sulfur compound and a preparation method thereof. The preparation method comprises the following steps: firstly adding a certain amount of basic ionic liquid into a reactor, then adding a sulfydryl reagent into the reactor, and sufficiently mixing the basic ionic liquid with the sulfydryl reagent for a certain time to makethe sulfydryl reagent and the basic ionic liquid react with each other to convert into alkyl sulfide negative ions; adding a certain amount of an addition receptor vinyl acrylate compound into the reactor, oscillating the reactor at a speed of 200rev. / min in a constant temperature oscillating box and monitoring the reaction process by using a TLC; when the reaction is completed, adding a certain volume of extracting agent into mixed solution to extract, after the extract liquid is combined, reducing pressure, distilling and recycling the extracting agent, and separating a crude product by a chromatographic column; or carrying out pressure reduction and distilling on the mixed solution after the reaction to obtain a product, wherein the residual basic ionic liquid is continuously used after being washed. The preparation method is carried out at room temperature, has good yield and has practical industrial operability.

Description

technical field [0001] The invention relates to compounds in the field of chemistry and a preparation method thereof, in particular to a method for preparing β-hydrocarbyl sulfur-substituted vinyl propionate sulfur-containing compounds by promoting the reaction of mercapto reagents and vinyl acrylate derivatives with an alkaline ionic liquid. technical background [0002] Many synthetic or natural sulfur-containing organic compounds are biologically active. Transition metal-catalyzed C-S bond synthesis reactions have opened up a new stage of development for organic sulfur chemistry. However, transition metal complexes generally have disadvantages such as difficult preparation, high price, easy loss, difficult recovery, and the production of substances harmful to the environment. These harmful substances will have a serious impact on the environment on which human beings depend for survival and human health. The increasingly prominent problem of environmental pollution urge...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C319/18C07C323/52C07D235/28
Inventor 娄凤文
Owner HUAIYIN TEACHERS COLLEGE
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