Hydrochloric Acid → 2-Acetyl-2-methylpropane-1,3-diol bismethanesulphonate

Participants

Reaction Steps

66 g (0.5 mol) of 3-oxo-2,2-bis-(hydroxymethyl)-butane (for the preparation, see Beilstein H 1, E III 3306, IV 4132 and J.Chem.Soc., London, 1932, 2671) were dissolved in 300 ml of 1,2-dichloroethane, 114.5 g (1 mol) of methanesulphonic acid chloride were added dropwise, and 158 g (2 mol) of pyridine were added dropwise at 0° to 5° C. The mixture was subsequently stirred at room temperature for 15 hours and then poured onto 600 ml of ice-water and 100 ml of concentrated hydrochloric acid. A solid thereby precipitated and was filtered off. The aqueous phase was extracted with 1,000 ml of methylene chloride; the solid was dissolved in the methylene chloride phase, the organic phase was dried over sodium sulphate, the solvent was distilled off under a waterpump vacuum and the residue was suspended in 200 ml of ether. The residue was filtered off and washed with 100 ml of ether. 100 g (about 70% of theory) of 2-acetyl-2-methylpropane-1,3-diol bismethanesulphonate of melting point 105°-108° C. were obtained. ##STR71##

Provenance & Evidence