反应详情

温度

-78 °C

A solution of n-butyllithium (1.6M, 72.50 mL, 0.116 mol) was added slowly dropwise to a solution of bromo-4-methoxymethoxybenzene (25.23 g, 0.116 mol) in dry THF (110 mL) at −78° C. After stirring for 50 min at −78° C., dichlorodiisopropylsilane (21.00 mL, 0.116 mol) was charged into the flask. The reaction mixture was slowly allowed to warm to room temperature with stirring. Diethyl ether (100 mL) was added, the mixture was then stirred for 15 min and filtered. The filtrate was concentrated in vacuo to an oil. The oil was purified by short path distillation (116-128° C./0.18 mm Hg) to afford the compound (23.7 g, 71%) as a slightly cloudy pale yellow oil.

1. temperatureto warm to room temperature
2. stirringwith stirring
3. stirringthe mixture was then stirred for 15 min
4. filtrationfiltered
5. concentrationThe filtrate was concentrated in vacuo to an oil
6. distillationThe oil was purified by short path distillation (116-128° C./0.18 mm Hg)