- Preparation of Triethyloxonium fluoborate
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Triethyloxonium fluoborate (CAS NO.: ), which is also known as , could be produced through the following synthesis route.
A 2-l. three-necked flask, a stirrer, a dropping funnel, and a condenser provided with a drying tube are dried in an oven at 110°, assembled while hot, and cooled in a stream of dry nitrogen. -dried ether (500 ml.) and 284 g. (252 ml., 2.00 moles) of freshly distilled boron fluoride etherate are placed in the flask. (140 g., 119 ml., 1.51 moles) is added dropwise to the stirred solution at a rate sufficient to maintain vigorous boiling (about 1 hour is needed). The mixture is refluxed an additional hour and allowed to stand at room temperature overnight. The stirrer is replaced by a filter stick, and the supernatant ether is withdrawn from the crystalline mass of triethyloxonium fluoborate; nitrogen is admitted through a bubbler during this operation to prevent atmospheric moisture from entering the flask. The crystals are washed with three 500-ml. portions of sodium-dried ether. The flask is transferred to a dry box, and triethyloxonium fluoborate is collected on a sintered-glass filter and bottled in a stream of dry nitrogen. The fluoborate is colorless; m.p. 91–92° (dec.), yield 244–272 g. (85–95%).
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