2,3-Difluorophenol ≥99.0%

2,3-Difluorophenol ≥99.0%

C₆H₄F₂O

CAS No.:6418-38-8

Chemical synthesis

Put 2.73 g (17.1 mmol) of 2,3-difluorophenylboronic acid in a 500 ml round-bottomed flask after dissolving it in diethyl ether. Dropwise add 10 milliliters (30 weight percent in water) of hydrogen peroxide to the agitated mixture. For one hour, the reaction mixture was refluxed. Room temperature was reached by cooling the reaction mixture. Diethyl ether was used to extract the crude product (100 ml). Brine (100 ml) and 10% aqueous ferrous ammonium sulfate solution (200 ml) were used to wash the crude product. Over MgSO4, the raw product was dried. Lower pressure was used to extract the solvent. The chemical 2,3-difluorophenol was obtained by vacuum distillation purification of the product. In Figure 1, the synthesis method is displayed.

100g (0.68mol) of 2,3,4-trifluoroaniline should be added dropwise while stirring at room temperature to a 1L polyethylene container fitted with a stirrer, thermometer, and cooling and heating bath after 600g (3.06mol) of 50% sulfuric acid has been added. Get a sulfate solution ready. To make a diazonium salt solution, add 173g (0.75 mol) of 30% sodium nitrite aqueous solution dropwise into the sulfate solution, reducing the liquid temperature to below 30°C. For two hours, the diazonium salt solution was heated to 50°C and stirred. A 2-liter polyethylene container fitted with a stirrer, thermometer, and cooling bath was filled with 177g (1.34mol) of 50% aqueous hypophosphorous acid solution. After finishing the heating and stirring, the diazonium salt solution is dropped while being stirred.

The heating and stirring processes are now complete, and the diazonium salt solution is added while the liquid temperature is cooled to a maximum of 50°C. The mixture was agitated for an additional hour at room temperature after the addition was finished. Use 500 milliliters of methylene chloride solvent for the extraction, let it evaporate, and then distill. It yields 2,3-difluorophenol. In Figure 2 [2], the synthesis method is displayed.

Packing, Storage, Handling and Transportation

3-Fluorophenol should be kept in dark place under inert atmosphere at room temperature.

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