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ChemicalBook CAS DataBase List 5-Fluoro-2-Methyl-3-nitrobenzoic acid

5-Fluoro-2-Methyl-3-nitrobenzoic acid synthesis

4synthesis methods
33184-16-6 Synthesis
5-Fluoro-2-methylbenzoic acid

33184-16-6
315 suppliers
$6.00/1g

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Yield: 70.5%

Reaction Conditions:

with sulfuric acid;nitric acid in dichloromethane at 30 - 40; for 3 h;Temperature;Reagent/catalyst;

Steps:

6 Preparation of 2-methyl-3-nitro-5-fluorobenzoic acid
30 g (0.195 mol) of 2-methyl-5-fluorobenzoic acid was added to a mixed solution of 30 ml of concentrated sulfuric acid and 150 ml of dichloromethane, and the mixture was heated to 30 ° C to 40 ° C with stirring.24.5 g (0.39 mol) of fuming nitric acid was added dropwise, and the temperature was controlled at 30-40 °C.After the completion of the dropwise addition, the reaction was carried out for 3 hours, the raw materials basically disappeared, the reaction was stopped, and the reaction solution was taken., pour into ice water. Filter, filter cake rinsed with water and drained. A wet product was obtained, dried at 50 ° C to give 30 g, HPLC 94%. The pure yield was 70.5%.

References:

Zhejiang Tianyu Pharmaceutical Co., Ltd.;Shanghai Xinbu Pharmaceutical Technology Co., Ltd.;Wang Xueyue;Li Gongyong;Chen Kexi CN108929217, 2018, A Location in patent:Paragraph 0080; 0084; 0086; 0087; 0088