反应详情

A mixture of 34.5 g (0.22 mol) of 6-fluoro-2-nitrotoluene, 30.7 g (0.22 mol) of potassium carbonate, 105.4 g (0.66 mol) of potassium permanganate and 3.3 liters of water is heated at 100° C. until the permanganate is decolorised (ca 2.5 hours). After cooling and removal of the unreacted 6-fluoro-2-nitrotoluene by extraction with ethyl acetate, the aqueous phase is adjusted to pH 1 with hydrochloric acid and extracted three times with ethyl acetate. The combined organic extracts are dried over magnesium sulphate and concentrated, there being obtained 6-fluoro-2-nitrobenzoic acid. After recrystallisation from ethyl acetate/n-hexane, the product melts at 146°-148° C.

1. custom(ca 2.5 hours)
2. temperatureAfter cooling
3. customremoval of the unreacted 6-fluoro-2-nitrotoluene
4. extractionby extraction with ethyl acetate
5. extractionextracted three times with ethyl acetate
6. dry with materialThe combined organic extracts are dried over magnesium sulphate
7. concentrationconcentrated