反应详情

33.5 g of a 30% strength methanolic solution of sodium methoxide were added to a solution of 3.0 g (9.3 mmol) of 3-chloro-2-(4-chloro-3-methoxyphenyl)-5-trifluoromethylpyridine in 100 ml of methanol. The mixture was refluxed for 20 h and then poured into about 500 ml of ice-water. The product was extracted from the aqueous phase with 3×100 ml of methylene chloride. The combined organic phases were dried over sodium sulfate and concentrated. The oily residue was induced to crystallize by trituration with n-hexane. Yield: 1.3 g of colorless crystals; melting point: 62°-63° C. (purity about 85%).

1. temperatureThe mixture was refluxed for 20 h
2. extractionThe product was extracted from the aqueous phase with 3×100 ml of methylene chloride
3. dry with materialThe combined organic phases were dried over sodium sulfate
4. concentrationconcentrated
5. customto crystallize by trituration with n-hexane