Heptane → 2-Chloro-2,4,4,6,6,8,8-heptamethyl-1,3,5,7,2,4,6,8-tetroxatetrasilocane

Participants

Reaction Conditions

Reaction Steps

To a 1000 mL three-necked round bottom flask equipped with a magnetic stirring bar, a thermometer, an inlet for gases and an outlet fitted with a drying tube, was charged the following: 37.17 g (77.87 mmol) of heptamethylcyclotetrasiloxane (59.2% in octamethylcyclotetrasiloxane) and 521.9 g (5214 mmol) of heptane. The mixture was cooled in an ice bath to 0° C. Chlorine (Cl2) was bubbled through the stirred mixture at a rate such that the temperature did not rise above 10° C. The addition of the chlorine was continued until a persistent yellow color, accompanied by a drop in temperature, was observed. Nitrogen gas was bubbled through the solution to remove the HCl generated in the reaction and the excess Cl2. A yield of 100% under anhydrous conditions was determined by gas chromatographic analysis.

Provenance & Evidence