ChemicalBook CAS DataBase List 2-Chloro-4-fluorobenzoic acid

2-Chloro-4-fluorobenzoic acid synthesis

6synthesis methods

Product Name:2-Chloro-4-fluorobenzoic acid
CAS Number:2252-51-9
Molecular formula:C7H4ClFO2
Molecular Weight:174.56

2-Chloro-4-fluorobenzoic acid is synthesized from m-chloroaniline in four steps. 1) m-Chloroaniline reacts with 2-(trimethylsilyl)ethoxymethyl chloride in the presence of potassium carbonate, potassium iodide, and ionic liquid to give N,N-bis(trimethylsil

84194-36-5 Synthesis

84194-36-5
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2252-51-9
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$7.00/5g

Yield:2252-51-9 90.8%

Reaction Conditions:

with hydrogenchloride;sodium chlorite in water;acetonitrile at 0 - 80; for 1 h;

Steps:

4.1 (1) Compound 21: Synthesis of 2-chloro-4-fluorobenzoic acid
Compound 17 (1 g, 6.31 mmol) and CH3CN (20 ml) were added to a 100 ml three-necked flask and stirred at 0°C until dissolved.Further, 5 ml of an aqueous solution of NaClO2 (1.71 g, 18.92 mmol) was added thereto, the mixture was further stirred and mixed, and 5 ml of an aqueous solution of HCl (3.31 ml, 25.23 mmol) was slowly added dropwise.After the addition was completed, the mixture was stirred at 0°C for 0.5 h. The reaction flask was transferred to a silicone oil bath, and the temperature was raised to 80°C and stirred for 0.5 h. The reaction was completed by TLC. The acetonitrile in the reaction solution was spin-dried and diluted with 10 ml of H2O.Adjust pH to 2 with 6N HCl, extract with ethyl acetate/water, dissolve the product in the organic phase, separate the liquid, collect the organic phase, dry with anhydrous Na2SO4, and spin dry the organic solvent.The crude product was obtained, purified by column chromatography, and eluted with petroleum ether:ethyl acetate=2:1 to give compound 21 as a white solid, 1.0 g, yield: 90.8%.

References:

Tianjin International Bio-pharmaceutical Joint Institute;Yang Cheng;Rao Zihe;Bai Cuigai;Sun Tao;Li Mingwei;Li Huiying;Li Xiaohui;Lu Jun;Zhao Xiujuan;Sun Tongyan CN107556289, 2018, A Location in patent:Paragraph 0099; 0101; 0102; 0103

FullText

201230-82-2 Synthesis