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A magnetically-stirred 70-mL fluoropolymer-lined steel autoclave was fitted with an internal thermocouple capable of determining the temperature of the liquid phase contained in the vessel, a pressure gauge, a pressure-relief valve, and a vent valve. The amine starting material, anhydrous or aqueous sodium 2-hydroxyethanesulfonate, and anhydrous or aqueous sodium hydroxide were charged to the open autoclave, which was then assembled and immersed in an electrically heated oil bath. With the vent valve closed, the stirred reaction mixture was rapidly heated to the reaction temperature and held at that temperature for the times specified in Examples 9, 10, and 13 below. The reaction mixture was then cooled to ambient temperature, the reactor opened, and the reaction product taken up in sufficient water to dissolve all solids.
EXAMPLE 1 Production of Sodium 2-bromoethane Sulfonate After 1018 g of 47% hydrobromic acid were added dropwise to 292 g of 60% aqueous sodium isethionate solution, the mixture was heated under reflux and 348 g were distilled off at normal pressure. The residue was cooled to 50 C. and 252 g of 47% hydrobromic acid were added, then further cooled from 50 C. to 5 C. The precipitated crystals were filtered out at about 5 C. and washed with 77.1 g of 47% hydrobromic acid being cooled to about 5 C. and then 17.5 g of water being cooled to about 5 C. The crystals were washed twice with a mixture of 408.6 g of acetone and 47.4 g of water being cooled to about 5 C., and further washed twice with 221 g of acetone being cooled to about 5 C. The crystals were dried under reduced pressure to afford 120 g of sodium 2-bromoethane sulfonate.
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