Synthesis of Methanesulfinyl Chloride

Set up a 50 mL RBF partially immersed in a dry ice-acetone bath to reach a temperature of -20°C, equipped with an addition funnel filled with 25 g of sulfuryl chloride, to the RBF add 5.44 g of dimethyl disulfide and 7 g of acetic acid. Start slow addition of the sulfuryl chloride and maintain the same temperature for 3h, thereafter strip the acetyl chloride formed as a by-product in a rotary evaporator. Distill the solution in a vacuum and collect the fraction which comes off at 44-45°C. The pure product should be stored under an inert gas at -10°C.

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The apparatus

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Distillation

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The pure product

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