- Preparation of n-Butyl sulfite
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n-Butyl sulfite (CAS NO.: ), which is also known as Butyl sulfite, could be produced through the following synthetic route.
In a 2-l. three-necked flask, fitted with a mercury-sealed stirrer, thermometer, condenser, and dropping funnel, is placed 684 g. (845 cc., 9.2 moles) of dry n-butyl alcohol. The condenser is connected to a trap for absorbing hydrogen chloride, and 500 g. (305 cc., 4.2 moles) of chloride is added over a period of two hours, with stirring. The reaction mixture is kept at 35–45°, by immersing the flask in ice water, during the addition of the first half of the thionyl chloride. After evolution of hydrogen chloride begins, the water bath is removed and a small flame applied to maintain this temperature. After all the thionyl chloride has been added the temperature is raised gradually to the boiling point, over a period of thirty minutes, to complete the reaction and remove the remainder of the hydrogen chloride. The reaction mixture is then transferred to a 1-l. modified Claisen flask with a 25-cm. fractionating side arm, and fractionated under diminished pressure. After a fore-run consisting largely of unchanged alcohol, there is obtained 625–689 g. (77–84 per cent of the calculated amount) of n-butyl sulfite, b.p. 109–115°/15 mm. Refractionation gives 585–674 g. (72–83 per cent) of a product distilling at 109–112° at 14 mm.
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