2,2-dimethyloxasilinane

Conditions: temp:100.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: 523.8 g. 1,1-dimethyl-1-sila-2-oxacyclohexane (4.0 moles), 304.7 g. acrylic acid (4.2 moles), 1.0 g. hydroquinone, 13.5 ml concentrated sulfuric acid, and 1200 ml cyclohexane are measured into a 3 liter reactor. The mixture is stirred during heating. The mixture is heated with steam (100° C.) and kept under dry air. Water formed during the reaction is removed continuously as the cyclohexane and water azeotrope. After 6 hrs. of heating, 31.9 ml water is collected and heating is stopped. The solution is then column filtered over 1 kg. activated alumina and filtered again over 740 g. grade 12 silica gel. The cyclohexane is removed from the product by rotary evaporation at reduced pressure. 1,3-bis (4-acryloxy butyl) tetramethyl disiloxane is obtained. The product is 98.3% pure by gas chromatography. The identity of the product is confirmed by infrared spectrum and elemental analysis. The analysis results are 55.96% C, 9.26% H, and 13.85% Si. during heating under dry air Water formed during the reaction is removed continuously as the cyclohexane and water of heating 31.9 ml water is collected heating column filtered over 1 kg filtered again over 740 g The cyclohexane is removed from the product by rotary evaporation at reduced pressure