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ChemicalBook CAS DataBase List 2-Amino-5-chlorobenzophenone
719-59-5

2-Amino-5-chlorobenzophenone synthesis

9synthesis methods
5-CHLORO-3-PHENYLANTHRANIL

719-64-2

2-Amino-5-chlorobenzophenone

719-59-5

(2) 10.0 g of intermediate (II) was added to a three-necked flask containing 50 mL of ethanol, 4.8 g of iron powder was added, and refluxed for 0.5 hours. Subsequently, 1 mL of 6 mol/L sulfuric acid solution was slowly added dropwise. After the dropwise addition, the reaction was continued to reflux for 1 hour. After the reaction was completed, the pH of the reaction solution was adjusted to 8 with NaOH solution and cooled to 50 °C. Add 0.2 g of activated carbon and reflux for 0.5 h. Perform hot filtration into a crystallization flask and cool the crystals. The crystals were washed with ethanol and dried to give 9.60 g of intermediate (III) in 95.1% yield, melting point 96.3-98.2 °C.

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Yield:719-59-5 95.1%

Reaction Conditions:

Stage #1: 5-chloro-3-phenylanthranilwith iron in ethanol; for 0.5 h;Reflux;
Stage #2: with sulfuric acid in ethanol; for 1 h;Reflux;

Steps:

2.2

(2) Take 10.0g of intermediate (II) into a three-necked bottle.50ml ethanol, 4.8g iron powder,After refluxing for 0.5 h, 1 ml of sulfuric acid (6 mol/L) was added dropwise.After the completion of the dropwise addition, the reaction was refluxed for 1 h.After the reaction is completed, a NaOH solution is added to adjust the pH to 8,Cool down to 50 ° C, add 0.2g activated carbon,Reflux for 0.5h,Thermal filtration into the crystallization bottle, cooling and crystallization,Ethanol washing, drying to obtain intermediate (III) 9.60g, The yield is 95.1%.The melting point is 96.3-98.2 °C.

References:

CN108250091,2018,A Location in patent:Paragraph 0032; 0034; 0040

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