Methyl sulfinate (CAS NO.: ), with other names as , , could be produced through the following synthetic routes.

In a 5-l., three-necked, round-bottomed flask equipped with a sealed mechanical stirrer and a reflux condenser carrying a drying tube are placed 54.6 g. (0.25 mole) of diphenyl disulfide, 450 ml. of chloroform, and 450 ml. of methanol. To the stirred solution at the reflux temperature is added 443.4 g. (1.00 mole) of tetraacetate in 2 l. of chloroform during 8 hours. Owing to formation of , the initially yellow solution becomes dark brown during the addition. The mixture is kept at the reflux temperature overnight (about 12 hours), after which 2 l. of chloroform is removed by distillation at atmospheric pressure. The mixture then is cooled to room temperature, and 330 ml. of distilled water is added with stirring to decompose any excess lead tetraacetate. Lead dioxide is removed by filtration of the entire mixture using a Celite®-coated filter paper. The chloroform layer is washed with distilled water until the washings are free of lead ions. The chloroform solution is dried over anhydrous magnesium sulfate and, after separation of the drying agent, is concentrated by means of a rotating-flask evaporator. The oily yellow residue is left overnight under vacuum (about 0.1 mm.) to remove any traces of hexachloroethane. Distillation is effected through a 15-cm. Vigreux column under reduced pressure. The yield of methyl benzenesulfinate is 48.6–53 g. (62–68%), b.p. 59–60° (0.04 mm.), 76–78° (0.45 mm.); n²⁵D 1.5410–1.5428, reported n²⁰D 1.5400,3 1.5440.

Notice: Care should be taken to keep methyl benzenesulfinate off the skin.