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34649-01-9

Benzoic acid, 2-(acetylamino)-5-chloro-4-nitro- synthesis

3synthesis methods
-

Yield:34649-01-9 68.2%

Reaction Conditions:

with potassium permanganate;water;magnesium sulfate at 80; for 1.75 h;

Steps:

48.3 2-Acetamido-5-chloro-4-nitrobenzoic acid

N - (2-methyl-4-chloro-5-nitrophenyl) acetamide(15.34 g, 67.1 mmol)Was added to a 6711 aqueous solution of magnesium sulfate (10.11g, 84.0mmol) and potassium permanganate (29.22g, 184.9mmol), and the temperature was raised to 80 ° CAfter 45 min, magnesium sulfate (5.08 g, 42.2 mmol) and potassium permanganate (14.63 g, 92.6 mmol) were added and reacted for 1 h. Filtration, filtrationThe cake was washed with hot water (2 X 300 mL). The filtrate was acidified with 3. ON HC1 solution to pH 3.0, 300 mL of dichloromethane was added to the solution,Extracted with dichloromethane (2 x 200 mL), the combined methylene chloride solutions were dried over anhydrous magnesium sulfate, concentrated to dryness under reduced pressure,To give 11.84 g of yellow solid 2-acetamido-5-chloro-4-nitrobenzoic acid in a yield of 68.2%.

References:

CN103382182,2016,B Location in patent:Paragraph 0589; 0591; 0596; 0597