反应详情

温度

100 °C

38.5 g of sodium perborate tetrahydrate were added in portions over the course of 30 minutes to a solution of 16.0 g of 3-chloro-2-(4-chloro-3-formylphenyl)-5-trifluoromethylpyridine in 100 ml of glacial acetic acid at 100° C., followed by stirring at 100° C. for 1.5 hours. The mixture was cooled and then poured into 400 ml of water. The product was extracted from the aqueous phase with 3×100 ml of tert-butyl methyl ether. The combined organic phases were dried over sodium sulfate and then concentrated. The residue was triturated with n-hexane. The material insoluble in hexane was removed and extracted by boiling twice with ether, the pyridine N-oxide byproduct remaining undissolved. The combined ether phases were dried over sodium sulfate and concentrated to result in 13.7 g (81%) of colorless crystals; melting point: 149°-151° C.

1. temperatureThe mixture was cooled
2. extractionThe product was extracted from the aqueous phase with 3×100 ml of tert-butyl methyl ether
3. dry with materialThe combined organic phases were dried over sodium sulfate
4. concentrationconcentrated
5. customThe residue was triturated with n-hexane
6. customThe material insoluble in hexane was removed
7. extractionextracted
8. dry with materialThe combined ether phases were dried over sodium sulfate
9. concentrationconcentrated