Methylene bis(chlorosulfate) → Methanediol, 1,1-dimethanesulfonate

Participants

Reaction Steps

In dimethyl carbonate (10 mL), methylene bis(chlorosulfate) [CISO2OCH2OSO2Cl] (1.5 g, 6.1 mmol) synthesized on the basis of the method described in U.S. Pat. No. 4,649,209 was reacted with methanesulfonic acid pyridinium salt (2.1 g, 12.0 mmol) under agitation at 55° C. for 3 hours. After the reaction was completed, precipitated chlorosulfonic acid pyridinium salt was separated through filtration, and concentration was performed under reduced pressure, so as to obtain a light brown solid. An adsorption treatment with activated carbon was performed and, thereafter, refining was performed through recrystallization, so as to obtain a desired product, methylene bis(methanesulfonate), at a yield of 48% (0.6 g, 2.9 mmol). The measurement result of 1H NMR is as described below.

Provenance & Evidence