反应详情

2.1 g of 5% palladium carbon was added to a methanol 200 ml solution of 24.8 g (58.1 mmol) of (2,3,4-trimethoxy-6-methylphenyl)(2,3-dichloro-5-trifluoromethyl-4-pyridyl)methanol obtained in Step (a) and 9.50 ml (68.2 mmol) of triethylamine, followed by stirring under hydrogen atmosphere for 4 hours. The mixture was subjected to filtration, 50 ml of water was added, and methanol was distilled off under reduced pressure. The aqueous layer was extracted with ethyl acetate, and 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 15.9 g (yield: 70%) of (2,3,4-trimethoxy-6-methylphenyl)(3-chloro-5-trifluoromethyl-4-pyridyl)methanol (melting point: 102 to 105° C.).

1. filtrationThe mixture was subjected to filtration, 50 ml of water
2. additionwas added
3. distillationmethanol was distilled off under reduced pressure
4. extractionThe aqueous layer was extracted with ethyl acetate
5. dry with materialthe organic layer was dried over anhydrous sodium sulfate
6. filtrationsubjected to filtration
7. distillationthe solvent was distilled off under reduced pressure
8. customThe crude product was purified by silica gel column chromatography