反应详情

A mixture of 5.22 g of 2-hydroxy-3-nitro-5-(trifluoromethyl)pyridine, 4.2 g of phosphorus oxychloride and 2.0 g of quinoline was refluxed with heating for 5.5 hours. The reaction mixture was cooled down to room temperature, then, the reaction mixture was poured into ice water. This mixture was neutralized with a sodium hydroxide aqueous solution, then, the mixture was extracted with ethyl acetate twice. The combined organic layers were washed with water and saturated saline, dried over magnesium sulfate, then, concentrated under reduced pressure. The residue was subjected to silica gel column chromatography, to obtain 4.88 g of 2-chloro3-nitro-5-(trifluoromethyl)pyridine.

1. temperaturewas refluxed
2. temperaturewith heating for 5.5 hours
3. extractionthe mixture was extracted with ethyl acetate twice
4. washThe combined organic layers were washed with water and saturated saline
5. dry with materialdried over magnesium sulfate
6. concentrationconcentrated under reduced pressure