Dimethyl Carbonate → Methylene bis(4-methoxybenzenesulfonate)

Participants

Reaction Steps

In dimethyl carbonate (30 mL), methylene bis(chlorosulfate) [CISO2OCH2OSO2Cl] (4.5 g, 13 mmol) was reacted with 4-methoxybenzenesulfonic acid pyridinium salt (7 g, 26 mmol) under agitation at 55° C. for 2 hours. After the reaction was completed, precipitated chlorosulfonic acid pyridinium salt was separated through filtration. Washing with water was performed and, subsequently, concentration was performed under reduced pressure, so as to obtain a pale red transparent oil. Refining was performed through recrystallization, so as to obtain a desired product, methylene bis(4-methoxybenzenesulfonate), at a yield of 32% (1.65 g, 4.2 mmol). The measurement result of 1H NMR is as described below.

Provenance & Evidence