反应详情

To a mixture of 66.60C (0.38 g, 1.3 mmol), 1-bromo-3-methylbut-2-ene (commercially available from Aldrich) (0.31 mL, 2.6 mmol) and sodium iodide (0.40 g, 2.6 mmol) in DMF (8 mL), was added indium (0.30 g, 2.6 mmol). The resulting mixture was stirred at room temperature for 1 hour and then additional 1-bromo-3-methylbut-2-ene (100 mg) and indium (100 mg) were added and the mixture was stirred at room temperature for one more hour. The reaction was quenched with water (20 mL) and extracted with EtOAc (200 mL). The organic phase was washed with brine, dried over anhydrous sodium sulfate, and filtered. After removing solvent, the residue was purified by flash chromatography (silica gel, 1:4 EtOAc/hexane) and gave product (66.60D), in 94% yield.

1. stirringthe mixture was stirred at room temperature for one more hour
2. customThe reaction was quenched with water (20 mL)
3. extractionextracted with EtOAc (200 mL)
4. washThe organic phase was washed with brine
5. dry with materialdried over anhydrous sodium sulfate
6. filtrationfiltered
7. customAfter removing solvent
8. customthe residue was purified by flash chromatography (silica gel, 1:4 EtOAc/hexane)