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Synthesis method for paranitrobenzoyl chloride

A technology of nitrobenzoyl chloride and p-nitrobenzoic acid, which is applied in the field of synthesis of p-nitrobenzoyl chloride, can solve the problem of not finding detailed literature on nitrobenzoyl chloride, and avoid the recovery of solvents and materials , high purity, and the effect of reducing production costs

Inactive Publication Date: 2012-11-28
SHANDONG KAISHENG NEW MATERIALS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, in the relevant information on the preparation of this product, there is no detailed literature on the production process of p-nitrobenzoyl chloride prepared by the reaction of thionyl chloride and p-nitrobenzoic acid.

Method used

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  • Synthesis method for paranitrobenzoyl chloride

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Add 33.5g of p-nitrobenzoic acid, 0.3g of benzyltriethylammonium chloride, and then add 95g of thionyl chloride into the reaction flask, stir evenly, heat to 80°C, and keep the temperature for 16 hours. Excessive thionyl chloride was distilled under reduced pressure to obtain 36.27g of the product, the chromatographic content was 99.84%, and the yield was 97.50%.

Embodiment 2

[0026] Add 50g of p-nitrobenzoic acid, 0.075g of benzyltriethylammonium bromide, 125g of thionyl chloride into the reaction flask, stir evenly, heat to 80°C, and keep it warm for 15 hours. After the reaction is over, evaporate excess chlorine sulfoxide, then vacuum distillation to obtain product 54.12g, the chromatographic content is 99.85%, and the yield is 97.48%.

Embodiment 3

[0028] Add 100g of p-nitrobenzoic acid, 0.1g of benzyltriethylammonium bromide, and 200g of thionyl chloride into the reaction flask, stir well, heat to 85°C, keep warm for 13 hours, and when the reaction is over, evaporate excess chlorine sulfoxide, then vacuum distillation to obtain product 109.47g, the chromatographic content is 99.74%, and the yield is 98.58%.

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Abstract

The invention relates to a synthesis method for paranitrobenzoyl chloride and belongs to the field of fine chemical industry. The method is characterized by comprising the following steps: directly reacting p-nitrobenzoic acid with sulfoxide chloride under the catalytic action of quaternary ammonium salt; distilling and recovering the residual sulfoxide chloride; and distilling under reduced pressure to obtain high-purity paranitrobenzoyl chloride. The sulfoxide chloride serves as an acyl chlorination reagent and a solvent and organic solvents such as carbon tetrachloride are not required, so recycling of solvents and materials and energy loss are avoided, the obtained product has high purity and does not need to be refined, the chromatograph content of the product obtained by primary distillation can reach over 99.5 percent, production cost is reduced, the yield of equipment is increased, blockage of pipelines is avoided, and burden is reduced for the subsequent procedure.

Description

technical field [0001] The invention relates to a synthesis method of p-nitrobenzoyl chloride, which belongs to the field of fine chemicals. Background technique [0002] p-Nitrobenzoyl chloride is an important intermediate in the synthesis of folic acid, procaine hydrochloride, N-p-aminobenzoyl-L-glutamic acid and other vitamin pharmaceutical products, and is also widely used in the production of pigments and color developers . Especially in recent years, with the rise of feed industry and the development of information industry, the consumption of p-nitrobenzoyl chloride is increasing. [0003] The existing production process of p-nitrobenzoyl chloride roughly has the following several types: ① Phosgene method: it is obtained by reacting p-nitrobenzoic acid and phosgene. Phosgene is a highly toxic substance, which is easy to cause harm to personnel and the environment. Hazard; ②Phosphorus pentachloride method, sulfur-chlorine method: These two methods are the effect of s...

Claims

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Application Information

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IPC IPC(8): C07C205/57C07C201/12
Inventor 张振霞张善民杨德耀李文娟贾远超薛居强孙丰春王志亮刘建村张勉志
Owner SHANDONG KAISHENG NEW MATERIALS
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