反应详情

16.4 g (304 mmol) of sodium methoxide was added to a toluene 150 ml solution of 18.5 g (47.5 mmol) of 4-(2,3,4-trimethoxy-6-methylbenzoyl)-3-chloro-5-trifluoromethylpyridine obtained in Step (c) and 16.6 ml (95.4 mmol) of hexamethylphosphorous triamide, followed by stirring under reflux with heating for 30 minutes. Water was added to terminate the reaction, and the aqueous layer was extracted with ethyl acetate. 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 11.7 g (yield: 64%) of 4-(2,3,4-trimethoxy-6-methylbenzoyl)-3-methoxy-5-trifluoromethylpyridine (melting point: 103 to 106° C.).

1. temperatureunder reflux
2. temperaturewith heating for 30 minutes
3. customto terminate
4. customthe reaction
5. extractionthe aqueous layer was extracted with ethyl acetate
6. dry with materialThen, the 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