Preparation method of p-anisoyl chloride

A technology of methoxybenzoyl chloride and methoxybenzoic acid, applied in the field of organic synthesis, can solve the problems of unsuitability for industrial production, high reaction conditions, long reaction time, etc., and achieves easy operation, high purity and mild reaction. Effect

A technology of methoxybenzoyl chloride and methoxybenzoic acid, applied in the field of organic synthesis, can solve the problems of unsuitability for industrial production, high reaction conditions, long reaction time, etc., and achieves easy operation, high purity and mild reaction. Effect

CN105461550AInactive Publication Date: 2016-04-06ZHEJIANG ESIGMA BIOTECH CO LTD
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  • Preparation method of p-anisoyl chloride

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Experimental program
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Effect test

Embodiment 1

[0019] Add 15.23g (0.1mol) of p-methoxybenzoic acid, 30.5g of dichloroethane, and 0.3g (0.004mol) of DMF into the reaction vessel of the tail gas absorption device equipped with water, raise the temperature to 40°C, and slowly drop Add BTC-C with a concentration of 2mol / L 2 h 4 Cl 2 The solution was 15.5ml, and after the dropwise addition, the reaction was refluxed for 1 hour. After the solvent was recovered by distillation under reduced pressure, 16.88g of p-methoxybenzoyl chloride was obtained, the content was 99.62% (gas chromatography), and the yield was 98.57%.

Embodiment 2

[0021] Add 15.23g (0.1mol) of p-methoxybenzoic acid, 45.7g of dichloroethane, and 0.48g (0.006mol) of pyridine into the reaction vessel of the tail gas absorption device equipped with water, raise the temperature to 42°C, and slowly drop Add BTC / C with a concentration of 2mol / L 2 h 4 Cl 2 The solution was 15.5ml, and after the dropwise addition, the reaction was refluxed for 1.5 hours. After the solvent was recovered by distillation under reduced pressure, 16.86g of p-methoxybenzoyl chloride was obtained, the content was 99.68% (gas chromatography), and the yield was 98.28%.

Embodiment 3

[0023] Add 15.23g (0.1mol) of p-methoxybenzoic acid, 60.9g of dichloroethane, and 0.38g (0.005mol) of DMF into the reaction vessel of the tail gas absorption device equipped with water, raise the temperature to 45°C, and slowly drop Add BTC / C with a concentration of 2mol / L 2 h 4 Cl 2 The solution was 15.5ml, and after the dropwise addition, the reaction was refluxed for 2 hours. After the solvent was recovered by distillation under reduced pressure, 16.92g of p-methoxybenzoyl chloride was obtained, with a content of 99.87% (gas chromatography), and a yield of 98.82%.

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Abstract

The invention provides a preparation method of p-anisoyl chloride, and belongs to the technical field of carbon compounds. The method comprises the steps that p-anisic acid serves as the raw material, BTC / C2H4Cl2 serves as a reagent of sulfonyl chlorination, an initiator is added, a reaction is conducted at the reflux temperature, and the p-anisoyl chloride is prepared. According to the preparation method of the p-anisoyl chloride, the reaction condition is mild, the technology is simple, operation is easy, the purity and yield of obtained products are high, and the preparation method of the p-anisoyl chloride is suitable for industrial production.

Description

technical field [0001] The invention belongs to the technical field of organic synthesis, in particular to a preparation method of p-methoxybenzoyl chloride. Background technique [0002] p-Methoxybenzoyl chloride (4-Methoxybenzoylchloride), also known as anisyl chloride, 4-methoxybenzoyl chloride. Its structural formula is as follows: [0003] [0004] p-Methoxybenzoyl chloride is soluble in acetone, dichloromethane and benzene, and decomposes when it meets water or ethanol. Intermediates of drugs such as ketone and benzbromarone. [0005] At present, the generally known process for preparing p-methoxybenzoyl chloride is: reflux reaction with p-methoxybenzoic acid and thionyl chloride for 6 hours, recover thallus chloride, and obtain pure p-methoxybenzoyl chloride by distillation under reduced pressure. Benzoyl chloride produces a large amount of by-products hydrogen chloride and sulfur dioxide during the reaction. The method has a long reaction time, unsatisfactory ...

Claims

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Application Information

Patent Timeline
06 Apr 2016
Publication
CN105461550A
IPC
C07C65/21; C07C51/60
CPC
C07C51/60; C07C65/21
Inventors
吴中华; 张小朋