Diethyl Ether → HCID 178504336, compound

Participants

Reaction Steps

A 1 liter four-necked flask equipped with a reflux tube, a thermometer and a dropping funnel was thoroughly purged with nitrogen and dried. To the flask, fluorene (5.00 g, 30 mmol) and dehydrated ether (100 ml) were introduced and, then, a hexane solution of n-butyllithium (30 mmol) was dropwise added at −10° C. with stirring over a period of 30 minutes. After the dropwise addition of the hexane solution, the temperature of the system was allowed to spontaneously and slowly rise to room temperature, followed by stirring at room temperature for 4 hours. The reaction liquid became a yellow slurry. Them, the slurry was dropwise added to a dichlorodimethylsilane (18.24 ml, 150 mmol)/dehydrated ether (100 nl) solution at −10° C. with stirring over a period of 1 hour. The temperature of the system was allowed to spontaneously rise to room temperature, followed by stirring over night. The reaction solution was filtered under pressure through a glass filter (G-5) to remove lithium chloride, and the solvent and the unreacted dichlorodimethylsilane remained in the filtrate were removed under reduced pressure. The resultant product was reslurried with dehydrated ether (100 ml) and the obtained slurry was filtered under pressure through a glass filter (C-5) to obtain 3.30 g of a white powder (yield: 43%).

Provenance & Evidence