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ChemicalBook CAS DataBase List 4-Amino-3-methylbenzoic acid

4-Amino-3-methylbenzoic acid synthesis

6synthesis methods
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Yield:2486-70-6 96.1%

Reaction Conditions:

with palladium on activated charcoal;hydrogen in methanol at 60; under 5250.53 Torr; for 10 h;Autoclave;Temperature;Pressure;

Steps:

1; 2; 3; 4 Preparation of 3-methyl-4-aminobenzoic acid:
Add 1.0 mol of 3-methyl-4-nitrobenzoic acid, 1.2L of methanol, and 4g of catalyst into the 2L first autoclave, and close the lid of the autoclave after stirring evenly. Then replace it with nitrogen 3 times, and replace it with hydrogen 3 times, control the hydrogen pressure to 0.7 MPa, and adjust the stirring speed in the autoclave to 250 revolutions per minute and the temperature to 60°C. After continuing to stir the reaction for 10 hours, TLC tracked the spot plate. After the reaction, the catalyst was removed by filtration. The reaction liquid in the first autoclave was recovered under reduced pressure at 50° C. until no liquid flowed out. The brown solid intermediate I was obtained by drying. The mass was 145.3 g and the yield was 96.1%. The catalyst is palladium on carbon, and the intermediate I is 3-methyl-4-aminobenzoic acid.

References:

Zhejiang Jinliyuan Pharmaceutical Co., Ltd.;Fan Qingming;Chen Weiliang;Wang Chun;Zhao Binfeng;Sheng Kaiman CN111689903, 2020, A Location in patent:Paragraph 0029-0034; 0043-0046; 0055-0058; 0067-0070

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