反应详情

To a degassed solution of 4-iodobenzotrifluoride (4.70 g, 17.2 mmol), anilinium hypophosphite (3.51 g, 22.1 mmol), and 3-aminopropyl triethoxysilane (4.88 g, 22.1 mmol) in anhydrous acetonitrile (110 mL) were added palladium acetate (82.5 mg, 0.367 mmol, 2 mol %) and 1,3-bis(diphenylphosphino)propane (167 mg, 0.404 mol, 2.2 mol %). The mixture was heated under reflux for 32 hrs, then cooled down to room temperature, diluted with ethyl acetate and hydrochloric acid (IM) 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 magnesium sulfate. The solvent was removed in vacuo and the residue was purified by column chromatography using 25 to 100% ethyl acetate in petroleum ether. Further purification by distillation afforded compound AZ1 (1.14 g) in 28% yield.

1. temperatureThe mixture was heated
2. temperatureunder reflux for 32 hrs
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 magnesium sulfate
7. customThe solvent was removed in vacuo
8. customthe residue was purified by column chromatography
9. customFurther purification
10. distillationby distillation
11. customafforded compound AZ1 (1.14 g) in 28% yield