反应详情

温度

-78 °C

1-Methylfluorene (3.2 g, 18.0 mmol) in 50 mL THF was charged with BuLi, 2.35M solution in hexanes (7.65 mL, 18.0 mmol) at -78° C. The reaction mixture was stirred for 2 hr at -78° C. then 2-bromo-1.3-dioxolane (3.6 g, 19.8 mmol) was added by a syringe. The reaction was monitored by TLC (silica, 10% ethyl acetate/hexane). The reaction mixture was stirred for 2 hr at room temperature then the THF was evaporated. The residue was dissolved in ethyl acetate. The solution was washed with water, dried over magnesium sulfate, treated with a coarse silica gel and Norit and evaporated to yield 4.8 g (96.6%) of the desired product.

1. stirringThe reaction mixture was stirred for 2 hr at room temperature
2. customthe THF was evaporated
3. dissolutionThe residue was dissolved in ethyl acetate
4. washThe solution was washed with water
5. dry with materialdried over magnesium sulfate
6. additiontreated with a coarse silica gel and Norit
7. customevaporated