反应详情

To a degassed solution of 1-iodo-3,5-bistrifluoromethylbenzene (10.0 g, 29.4 mmol), anilinium hypophosphite (5.62 g, 35.3 mmol) and 3-aminopropyl triethoxysilane (7.81 g, 35.3 mmol) in anhydrous acetonitrile (200 mL) were added palladium acetate (132 mg, 0.588 mmol, 2 mol %) and 1,3-bis(diphenylphosphino)propane (267 mg, 0.647 mol, 2.2 mol %). The mixture was heated under reflux overnight, then cooled down to room temperature, diluted with ethyl acetate and hydrochloric acid (1 M), and partitioned. The aqueous layer was further extracted with ethyl acetate and the combined extracts were washed with aqueous sodium hydrogen carbonate and brine, and dried over sodium sulfate. The volatiles were removed in vacuo, and the residue was purified by column chromatography using 30 to 70% ethyl acetate in petroleum ether to afford compound AZ3 (4.65 g) as a cloudy oil in 52% yield.

1. temperatureThe mixture was heated
2. temperatureunder reflux overnight
3. custompartitioned
4. extractionThe aqueous layer was further extracted with ethyl acetate
5. washthe combined extracts were washed with aqueous sodium hydrogen carbonate and brine
6. dry with materialdried over sodium sulfate
7. customThe volatiles were removed in vacuo
8. customthe residue was purified by column chromatography
9. customto afford compound AZ3 (4.65 g) as a cloudy oil in 52% yield