Preparation method of chlorophenyl acetic acid

A manufacturing method and chlorobenzene technology, which are applied in the preparation of nitrile, organic chemistry, etc., can solve the problems of high labor intensity of operators, many equipment and sites, etc., and achieve the effects of less pollution of three wastes, high efficiency, and simple process operation.

Active Publication Date: 2007-03-14
WUHAN YOUJI IND
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Problems solved by technology

Compared to the actual production process, the refining post-treatment process requires m

Method used

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  • Preparation method of chlorophenyl acetic acid
  • Preparation method of chlorophenyl acetic acid

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Embodiment 1

[0023] Put 707g (7.07mol) of 98% concentrated sulfuric acid and 471g of water into a 2000ml four-necked flask, and slowly add 693g (4.53mol) of 99.0% o-chlorophenylacetonitrile dropwise at 90 to 130°C. After the heat preservation reaction for 1 hour, About 260g of water was distilled off, and the reaction was further incubated at 130-150°C for 3 hours to stop (sampling and analysis by GC, o-chlorophenylacetic acid: 99.74%, o-chlorophenylacetonitrile: 0.12%). Add 500ml of water to make it miscible and then cool and crystallize to 35°C. Suction filtration, and the obtained crystals were washed once with 500ml of warm water; the crystals were dried at 30-40°C to obtain 738.0g of finished o-chlorophenylacetic acid. Content (GC): 99.94%; Ash: 0.10%; Moisture: 0.12%; Melting point: 94.8-95.8°C (literature value: 94-97°C); Yield: 95.4%.

Embodiment 2

[0025] 11.9kg (0.119kmol) of 98% concentrated sulfuric acid and 8kg of clear water were dropped into a 50L enamel reaction kettle; 13.0kg (0.085kmol) of 99.0% p-chlorophenylacetonitrile was slowly added dropwise, and the operation was the same as above. Sampling analysis (GC) at the end of the reaction: p-chlorophenylacetic acid 99.82%; p-chlorophenylacetonitrile 0.07%. Keep warm at 100-110°C, settle for 10-15 minutes, and release acid water. Add 10-15kg of clear water, stir and heat up to 90-100°C, cool to crystallize, and other operations are the same as above. The obtained wet acid is dehydrated and dried under vacuum at 90-100°C to obtain 13.8Kg of p-chlorophenylacetic acid as a finished product. Product analysis: content (GC) 99.96%; ash content 0.03%; moisture content 0.07%; melting point 91.5-92.5°C (documentation value: 90-93°C); yield: 95.2%.

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Abstract

The present invention provides process of preparing chloro phenyl acetic acid. The technological process includes the main steps of hydrolyzing corresponding o-chloro benzyl cyanide, p-chloro benzyl cyanide or m-chloro benzyl cyanide in sulfuric acid solution to obtain course chloro phenyl acetic acid product; steam stripping to eliminate organic impurities; water washing and drying. The technological process of the present invention is simple, stable, less pollutant and suitable for industrial production.

Description

technical field [0001] The present invention relates to the manufacture method of chemical product, especially the method for preparing chlorophenylacetic acid. Background technique [0002] Chlorophenylacetic acid such as o (p, m) chlorophenylacetic acid, which (they) is an important organic chemical fine chemical intermediate, o (p, m) chlorophenylacetic acid is an important chemical and pharmaceutical intermediate, O-chlorophenylacetic acid is mainly used for diclofenac (also known as diclofenac sodium) (Guangdong Chemical Industry, [1992] 3, 36; China Pharmaceutical Industry Journal, [1991] 9, 387 / [1979] 11, 14; Pharmaceutical Progress, [1989] 3, 20); it is a widely used potent anti-inflammatory and analgesic drug (The Am.S. of Medicine, [1986] 48, 29). p-Chlorophenylacetic acid can be used in spices, fungicides, and plant growth hormones (Chemical Times, [1998] 2, 11-15); it can also be used as an intermediate in organic synthesis to produce p...

Claims

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Application Information

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IPC IPC(8): C07C63/70C07C51/08
Inventor 毛利民吴晓慧黎明郭涛霍俊聂少春
Owner WUHAN YOUJI IND
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