反应详情

A solution of the tetrafluoro naphthalene, 6-bromo-1,1,2,2-tetrafluoro-1,2-dihydronaphthalene (4.74 g, 16.80 mmol) in THF (15 ml) was treated with 30% aqueous NH4OH (30 ml) and zinc (8.45 g, 130 mmol) and stirred under N2 for 24 hours at RT. The reaction was monitored by GC/MS for disappearance of the starting material and found to be complete. The solution was filtered, extracted with hexane (30 ml), and filtered through a short silica column (20 g). The hexane solution was evaporated in vacuo to afford an oil. This crystallized on cooling to room temperature to afford 2.62 g (95% yield) of product.

1. filtrationThe solution was filtered
2. extractionextracted with hexane (30 ml)
3. filtrationfiltered through a short silica column (20 g)
4. customThe hexane solution was evaporated in vacuo
5. customto afford an oil
6. customThis crystallized
7. temperatureon cooling to room temperature