反应详情

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 methanesulphonyl chloride were added dropwise and 158 g (2 mol) of pyridine were added dropwise at 0° to 5° C. The reaction mixture was stirred for a further 15 hours at room temperature and the batch was then introduced into 600 ml of ice-water and 100 ml of concentrated hydrochloric acid. A solid precipitated out and this was filtered off. The aqueous phase was extracted with 1 liter 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. 100 g (about 70% of theory) of 2-acetyl-2-methyl-propane-1,3-diol bismethanesulphonate with a melting point of 105° to 108° C. were obtained. ##STR12##

1. customA solid precipitated out
2. filtrationthis was filtered off
3. extractionThe aqueous phase was extracted with 1 liter of methylene chloride
4. dissolutionthe solid was dissolved in the methylene chloride phase
5. dry with materialthe organic phase was dried over sodium sulphate
6. distillationthe solvent was distilled off under a waterpump vacuum