Nitrogen → HCID 178504156, compound

Participants

Reaction Conditions

Reaction Steps

A 300-mL, three-neck, round-bottom flask, which has a thermometer and N2 gas inlet and is equipped with a Teflon-covered magnetic stirring bar, is charged with methylphenylsulfone (7 g, 50 mmol) and diphenylsulfide (9.3 g, 50 mmol). The reaction mixture is cooled to 0° C. Methanesulfonic acid (100 mL) is added to the reaction vessel. The temperature is gradually raised to room temperature over a 30-min period. The reaction is continued for 20 h at room temperature. The reaction mixture is then poured into perchloric acid (60%, 100 mL) and stirred for 1 h at room temperature, and then water (100 mL) and dichloromethane (100 mL) were added. The aqueous layer is extracted with dichloromethane (2×50 mL). The organic layer is dried over anhydrous sodium sulfate. After evaporation, a residue is purified by recrystallization with ether. The solid is dried under vacuum at room temperature for 20 h.

Provenance & Evidence