5,5-dimethyl-1,3,2$l^{6}-dioxathiane-2,2-dione synthesis

Yield:1755-97-1 99%

Reaction Conditions:

with sodium hypochlorite;ruthenium trichloride in dichloromethane;water;isopropyl alcohol;

Steps:

2.b Production of 5,5-dimethyl-1,3,2-dioxathiane-2,2-dioxide

(b) with sodium hypochlorite: 10.0 g (0.064 mol) of 5,5-dimethyl-1,3,2-dioxathiane-2-oxide was introduced at 20° C. in 100 ml of methylene chloride and 50 ml of water in a 250 ml three-necked flask. 0.02 g of 90 percent ruthenium trichloride was added as a catalyst. 152.45 g (0.0727 mol) of sodium hypochlorite in water was added with stirring for 20 minutes, and the temperature increased to 30° C. The reaction mixture was stirred for five more hours and mixed with 10 drops of isopropanol; the yellow color faded and a black precipitate formed. The water phase was extracted twice with methylene chloride (50 ml), and the combined organic phases were extracted with NaHCO₃ solution (100 ml), dried with Na₂ SO₄ and concentrated by evaporation. The white crystalline product was dried overnight at room temperature at a pressure of 15 mbars and weighed 10.65 g, which corresponded to a yield of 99 percent, relative to the 5,5-dimethyl-1,3,2-dioxathiane-2-oxide used.

References:

US5159100,1992,A