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Synthesis technology of m-toluoyl chloride

A technology of m-toluoyl chloride and m-toluoyl chloride, which is applied in the field of synthesis of m-toluoyl chloride, can solve the problems of high equipment and environmental requirements, inconvenient use, and difficult separation of impurities, and achieve The effect of convenient tail gas treatment, cost saving and simple process

Inactive Publication Date: 2016-02-17
SHANDONG KAISHENG NEW MATERIALS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] In the prior art, m-toluoyl chloride is mostly produced by reacting phosgene or triphosgene with m-toluic acid, but phosgene is a highly toxic drug, and the production operation process is dangerous, and the requirements for equipment and environment are also high. high, inconvenient to use
Another data report takes m-toluic acid as raw material, reacts with phosphorus oxychloride (or phosphorus pentachloride) to prepare m-toluoyl chloride, and the yield is 90%. On the one hand, the yield is low, and on the other hand On the one hand, the impurities are more difficult to separate, and the purity is lower

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Add 50g of m-toluic acid and 100g of dichloromethane into the reaction flask, stir evenly to make them fully dissolved, then slowly add 45.9g of thionyl chloride, and keep stirring at 20°C for 10 hours. After the reaction, the solvent and excess thionyl chloride were removed by distillation under normal pressure, and then 54.6 g of the product was obtained by distillation under reduced pressure, with a chromatographic content of 99.1% and a calculated yield of 96.2%.

[0020] The temperature of the vacuum distillation is 129°C and the pressure is -0.095MPa.

Embodiment 2

[0022] Add 60g of m-toluic acid, 50g of dichloroethane, and 70g of tetrahydrofuran into the reaction flask, stir evenly to make it fully dissolved, then slowly add 56.1g of thionyl chloride, and keep stirring at 30°C for 7 hours. After the reaction, the solvent and excess thionyl chloride were distilled off under normal pressure, and then distilled under reduced pressure to obtain 66.1 g of the product with a chromatographic content of 99.4% and a calculated yield of 97.0%.

[0023] The temperature of the vacuum distillation is 133° C., and the pressure is -0.095 MPa.

Embodiment 3

[0025] Add 80g of m-toluene, 60g of xylene, 50g of toluene, and 50g of chloroform into the reaction flask, stir evenly to make it fully dissolved, then slowly add 75.5g of thionyl chloride, and keep stirring at 35°C for 5 hours. After the reaction, the solvent and excess thionyl chloride were removed by atmospheric distillation, and then 87.7 g of the product was obtained by distillation under reduced pressure, with a chromatographic content of 99.2% and a calculated yield of 96.5%.

[0026] The temperature of the vacuum distillation is 126° C., and the pressure is -0.095 MPa.

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PUM

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Abstract

The invention belongs to the technical field of organic synthesis, and particularly relates to a synthesis technology of m-toluoyl chloride. The synthesis technology comprises the steps that m-toluic acid and sulfoxide chloride are reacted in organic solvent, and after the reaction is completed, p-toluoyl chloride is obtained after atmospheric distillation and reduced pressure distillation are conducted. According to the synthesis technology of the m-toluoyl chloride, the reaction condition is mild, the technology is simple, the cost is low, the solvent and the sulfoxide chloride can be recycled, tail gas is easy to treat, the whole technology reaction is rapid, the purity of the product obtained through distillation is high, and industrial production is easy.

Description

technical field [0001] The invention belongs to the technical field of organic synthesis, and in particular relates to a synthesis process of m-toluoyl chloride. Background technique [0002] M-toluoyl chloride is an important chemical raw material used in medicine, pesticides, photosensitive materials, dyes and other fields. With the rapid development of modern polymer chemistry and materials chemistry, it has gradually become one of the most popular research fields in the world, and its applications are becoming more and more extensive. [0003] In the prior art, m-toluoyl chloride is mostly produced by reacting phosgene or triphosgene with m-toluic acid, but phosgene is a highly toxic drug, and the production operation process is dangerous, and the requirements for equipment and environment are also high. High, inconvenient to use. Another data report takes m-toluic acid as raw material, reacts with phosphorus oxychloride (or phosphorus pentachloride) to prepare m-toluo...

Claims

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Application Information

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IPC IPC(8): C07C63/04C07C51/60C07C51/64
CPCC07C51/60C07C51/64
Inventor 杨德耀毕义霞张善民张泰铭宋立伟谢圣斌薛居强
Owner SHANDONG KAISHENG NEW MATERIALS
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