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ChemicalBook CAS DataBase List 3-Fluoro-4-methylbenzonitrile
170572-49-3

3-Fluoro-4-methylbenzonitrile synthesis

11synthesis methods
Benzeneacetic acid, 4-cyano-2-fluoro-, methyl ester

942282-44-2

3-Fluoro-4-methylbenzonitrile

170572-49-3

General procedure for the synthesis of 3-fluoro-4-methylbenzonitrile from methyl 2-(4-cyano-2-fluorophenyl)acetate: 1.0 g of methyl 2-(4-cyano-2-fluorophenyl)acetate was added to a 50 mL four-necked flask, followed by the addition of 0.19 g of water, 1.15 g of 95% anhydrous calcium chloride and 15 g of N,N-dimethylacetamide. The mixture was stirred and heated to 140°C to 145°C and the reaction was carried out for 20 to 24 hours (the progress of the reaction was monitored by HPLC to ensure >99% conversion). Upon completion of the reaction, the mixture was cooled to 60°C to 70°C and subsequently concentrated under reduced pressure. Finally, the product was purified by column chromatography to afford 0.62 g of 3-fluoro-4-methylbenzonitrile as a light yellow solid in 89.0% yield.

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Yield:170572-49-3 89%

Reaction Conditions:

with calcium chloride in N,N-dimethyl acetamide;water at 140 - 145;

Steps:

3 Example 3: Synthesis of 3-fluoro-4-methylbenzonitrile:

A 50 mL four-necked flask was charged with 1.0 g of methyl 2-fluoro-4-cyanophenylacetate, 0.19 g of water was added,1.15 grams of 95% anhydrous calcium chloride and 15 grams of N, N-dimethylacetamide, stirring warming,140 ~ 145 incubated for 20 to 24 hours (HPLC monitoring, the conversion rate> 99%),The mixture was cooled to 60-70 ° C, concentrated under reduced pressure and purified by column chromatography to give 3-fluoro-4-methylbenzonitrile and 0.62 g of a pale yellow solid in a yield of 89.0%.

References:

CN107673994,2018,A Location in patent:Paragraph 0063; 0064; 0065

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