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Synthetic method for high-purity 2-(benzoyl) benzoyl chloride

A technology of o-benzoylbenzoic acid and benzoyl chloride is applied in the synthesis field of high-purity 2-benzoyl chloride, can solve the problems of poor production process safety, high requirements on reaction equipment, low product quality, etc. The effect of high product yield and simple post-processing

Inactive Publication Date: 2018-06-15
江苏佳麦化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The above method is complicated to operate, consumes a lot of energy, the product quality is not high, and the post-processing is also relatively complicated. In addition, the requirements for the reaction equipment are relatively high, and the safety of the production process is poor.

Method used

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  • Synthetic method for high-purity 2-(benzoyl) benzoyl chloride
  • Synthetic method for high-purity 2-(benzoyl) benzoyl chloride

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Put 132g of thionyl chloride and 226g of o-benzoylbenzoic acid into a 1000ml four-necked reaction flask, stir evenly, then put in 0.68g of benzyltriethylammonium chloride, start to heat up to 50°C, and keep it warm for 4.5h Finally, TLC tracking shows that the raw material point disappears, the reaction is over, lower to normal temperature, add 340g of chloral, 11.3g of concentrated hydrochloric acid and 0.25g of sulfamic acid, start to heat up, keep warm for 2h after reaching 90°C, TLC tracking shows that the raw material point disappears, the reaction is over, lower to normal temperature, drop 5% liquid caustic soda to adjust the pH of the system, wait until the pH value is about 7, let stand, and separate the water layer. Start rectification to recover chloral (97.5-99°C), the recovery rate is 90%, after the recovery is completed, continue to raise the temperature to recover the middle distillate, the middle distillate includes chloral, water and a small amount of fin...

Embodiment 2

[0026] Put 132g of thionyl chloride and 198g of o-benzoylbenzoic acid into a 1000ml four-necked reaction flask, stir evenly, put in 0.68g of benzyltriethylammonium chloride, start to heat up to 70°C, and keep it warm for 2 hours , TLC tracking shows that the raw material point disappears, the reaction is over, lower to normal temperature, add 198g of chloral, 10g of concentrated hydrochloric acid and 0.20g of sulfamic acid, start to heat up, keep warm for 1h after reaching 105°C, TLC tracking shows that the raw material point disappears , the reaction is completed, lowered to normal temperature, and 5% liquid caustic soda is added dropwise to adjust the pH of the system. When the pH value is about 7, let stand and separate the water layer. Start rectification to recover chloral (97.2-102°C), the recovery rate is 92%. After the recovery is completed, continue to raise the temperature to recover the middle distillate, which includes chloral, water and a small amount of finished p...

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Abstract

The invention discloses a method for synthesizing 2-(benzoyl) benzoyl chloride. The method comprises the following steps: firstly, carrying out acylation reaction on o-benzoylbenzoic acid and thionylchloride under the action of a catalyst to prepare 3-chloro-3-phenylbenzofuranone; secondly, taking trichloroacetaldehyde as a solvent and carrying out ring-opening and molecular rearrangement reaction on the 3-chloro-3-phenylbenzofuranone and concentrated hydrochloric acid under the action of the catalyst to prepare a target product 2-(benzoyl) benzoyl chloride. The method disclosed by the invention has the advantages of mild reaction conditions, simple and safe operation, simple post treatment, few three wastes, high yield of a product (total yield is 95 percent or above) and suitability forindustrial production; the purity of the 2-(benzoyl) benzoyl chloride is 99.5 percent or above.

Description

technical field [0001] The invention relates to a method for synthesizing high-purity 2-(benzoyl)benzoyl chloride, which belongs to the technical field of fine chemical organic synthesis. Background technique [0002] 2-(benzoyl)benzoyl chloride is an important organic synthesis intermediate, molecular formula: C 14 h 9 ClO 2 , CAS: 22103-85-1, the structural formula is as follows: [0003] [0004] 2-(Benzoyl)benzoyl chloride is widely used in the synthesis of medicine, food, dyes, pesticides, auxiliary agents, etc. In China, 2-(benzoyl)benzoyl chloride is mainly used for the synthesis of benzoxazocin, diphthalide, 2-methylethoxybenzophenone, acridone, 3-phenylphthalide, Important pharmaceutical or chemical raw materials such as methyl phthaloylbenzoate. [0005] The method of industrially producing 2-(benzoyl) benzoyl chloride at present is mainly to react with phthalic anhydride and benzene under the participation of anhydrous aluminum trichloride to prepare o-ben...

Claims

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Application Information

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IPC IPC(8): C07C51/58C07C51/64C07C65/34
CPCC07C51/58C07C51/64C07D307/88C07C65/34
Inventor 徐松刘学峰汪港郭维成
Owner 江苏佳麦化工有限公司
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