Diethyl Ether → HCID 178504336, compound

Participants

Reaction Conditions

Reaction Steps

A 1 liter four-neck 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. Under stirring at -10° C., a hexane solution of n-butyllithium (30 mmol) was dropwise added over a period of 30 minutes. After the dropwise addition, 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. The slurry was dropwise added to a dichlorodimethylsilane (18.24 ml, 150 mmol)/dehydrated ether (100 ml) solution under stirring at -10° C. over a period of 1 hour. After the temperature of the system was allowed to spontaneously rise to room temperature, the reaction mixture was stirred over night. Lithium chloride was removed by means of pressure filteration of the resulting solution using a glass filter (G-5). Further the solvent and the unreacted dichlorodimethylsilane remained in the filtrate were removed under reduced pressure. The resulting filtrate was reslurried with dehydrated hexane (100 ml) and subjected to pressure filteration using a glass filter (G-5) to obtain a white powder (3.30 g, yield: 43%).

Provenance & Evidence