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ChemicalBook CAS DataBase List 5-Amino-2-chlorobenzoic acid
89-54-3

5-Amino-2-chlorobenzoic acid synthesis

6synthesis methods
2-Chloro-5-nitrobenzoic acid

2516-96-3

5-Amino-2-chlorobenzoic acid

89-54-3

General procedure for the synthesis of 5-amino-2-chlorobenzoic acid from 2-chloro-5-nitrobenzoic acid: 75 g of 2-chloro-5-nitrobenzoic acid, 59 g of iron powder, 800 mL of ethanol, 150 mL of water, and 115 g of ammonium chloride were added to a reaction flask equipped with a stirrer. The mixture was heated to 78-80°C and the reaction was refluxed for 5 hours. The progress of the reaction was monitored by thin layer chromatography (TLC, unfolding agent was petroleum ether/ethyl acetate=1:3) during the reaction. Upon completion of the reaction, the reaction mixture was filtered while hot and the solids were washed with 150 mL of hot ethanol. The filtrate was dried at 60°C to obtain the crude product. Subsequently, the crude product was dissolved in 400 mL of ethyl acetate and heated to reflux pulping for 2 hours. The mixture was cooled to 0~5°C in a salt bath and then naturally reduced to room temperature and crystallized for more than 30 minutes. The crystals were separated by centrifugation and washed with 50 mL of ethyl acetate. Finally, it was dried under reduced pressure at 50°C to give 60.7 g of yellow solid 5-amino-2-chlorobenzoic acid with 99.1% purity and 95.1% yield.

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Yield:89-54-3 95.1%

Reaction Conditions:

with iron;ammonium chloride in ethanol;water at 78 - 80; for 5 h;

Steps:

2 Example 2
To the reaction flask was added 75 g of 2-chloro-5-nitrobenzoic acid, 59 g of iron powder, 800 ml of ethanol, 150 ml of water, 115 g of ammonium chlorideHeated to 78 ~ 80° C reflux 5h,TLC (PE / EA: 1/3) After the reaction was monitored, the filtrate was filtered while hot, washed with 150 ml of hot ethanol, and the filtrate was reduced to dryness at 60 ° C to obtain a crude product,Add 400ml ethyl acetate heating reflux beating 2h,Naturally dropped to room temperature after the salt bath cooling to 0 ~ 5° C crystallization more than 30min,Centrifuged, washed with 50 ml of ethyl acetate and dried at 50 ° C under reduced pressure to give a yellow solid 60.7 g of 2-chloro-5-aminobenzoic acid, 99.1% purity and 95.1% yield.

References:

Shandong Boyuan Pharmaceutical Co., Ltd.;Zan Jinxing;Zhao Xiwei;Liu Maosheng CN106748721, 2017, A Location in patent:Paragraph 0029; 0030

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