反应详情

温度

112.5 °C

A mixture of 11.88 g (69.2 mmol) of 1-butylpyridinium chloride and 13.69 g (124.3 mmol) of dimethyl sulfite is stirred at 110-115° C. (temperature of the oil bath) for 72 hours under an inert-gas atmosphere (nitrogen) in a sealed reaction vessel with pressure valve for 1-1.5 bar above atmospheric pressure. The end of the reaction is determined by NMR measurement. The product is pumped off over the course of 5 hours in vacuo at 13.3 Pa and 115° C. (temperature of the oil bath), giving 15.51 g of 1-butylpyridinium methanesulfonate as a solid. The melting point is 91-92° C. The yield is 96.9%. The residual chloride content is less than 5 ppm. The product is investigated by means of NMR spectroscopy.

1. customin a sealed reaction vessel with pressure valve for 1-1.5 bar above atmospheric pressure
2. customis pumped off over the course of 5 hours in vacuo at 13.3 Pa and 115° C.