反应详情

1.8 ml (19 mmol) of phosphorus oxychloride was added at 0° C. to 4 ml of toluene and 8 ml of dimethylformamide, followed by stirring for 10 minutes, and then 4.0 g (10 mmol) of 4-(2,3,4-trimethoxy-6-methylbenzoyl)-3-methoxy-5-trifluoromethylpyridine-N-oxide was added, followed by stirring for 20 minutes. After stirring at room temperature for 2 hours, the reaction solution was charged into ice water to terminate the reaction. The aqueous layer was extracted with ethyl acetate, and then the organic layer was dried over anhydrous sodium sulfate and subjected to filtration, and the solvent was distilled off under reduced pressure. The crude product was purified by silica gel column chromatography to obtain 3.57 g (yield: 85%) of 4-(2,3,4-trimethoxy-6-methylbenzoyl)-2-chloro-3-trifluoromethyl-5-methoxypyridine (melting point 117 to 119° C.).

1. stirringby stirring for 20 minutes
2. stirringAfter stirring at room temperature for 2 hours
3. customto terminate
4. customthe reaction
5. extractionThe aqueous layer was extracted with ethyl acetate
6. dry with materialthe organic layer was dried over anhydrous sodium sulfate
7. filtrationsubjected to filtration
8. distillationthe solvent was distilled off under reduced pressure
9. customThe crude product was purified by silica gel column chromatography