3-Chloro-4-fluoroaniline synthesis

350-30-1

367-21-5

In a reaction vessel equipped with a mechanical stirrer and a reflux condenser tube, 0.83 mol of erbium chloride powder, 150 mL of an aqueous sodium bromide solution with a mass fraction of 22%, and 3-amino-3-(4-ethylphenyl)propionic acid with a mass fraction of 37% were added. The stirring speed was adjusted to 190 rpm and the reaction mixture was heated to 70 °C and maintained at this temperature for 130 minutes. Subsequently, 0.31 mol of 3-chloro-4-fluoronitrobenzene was slowly added dropwise for a controlled dropwise time of 110 minutes. After the dropwise addition was completed, the reaction temperature was raised to 85 °C and the reaction was refluxed for 4 hours. Upon completion of the reaction, 130 mL of aqueous potassium bisulfite solution with a mass fraction of 40% was added and then distilled under vacuum at 3.3 kPa to collect the 105-115 °C fraction. The resulting fraction was dissolved in 300 mL of 65% o-xylene solution, decolorized by molecular sieve and recrystallized in 87% mass fraction of 2-thiophene acetonitrile solution to finally obtain 41.49 g of 3-chloro-4-fluoroaniline in 92% yield.