Ammonia → HCID 17978705, compound

Participants

Reaction Steps

984 g of adduct (8 mol of Mbutyl (=butyl-Me2SiO0.5) and 1312 (8 mol) of hexamethyldisiloxane are initially introduced into a flask equipped with stirrer, thermometer, water separator, reflux condenser and nitrogen blanketing, admixed with 0.1% sulphuric acids and 0.05% perfluorobutanesulphonic acid, neutralized for 4 h at a bottom temperature of 70° C. with 20 g of calcined soda, 3 g of water and 0.5 g of 25% strength NH3 solution, distilled to 110° C., cooled and filtered. This gives 1950 g of a crude product consisting of 36% hexamethyldisiloxane, 47% 1,1,1,3,3-pentamethyl-3-butyldisiloxane and 17% 1,1,3,3-tetramethyl-1,3-dibutyldisiloxane, which, as result of fractional distillation, produces 810 g of 97%-pure 1,1,1,3,3-pentamethyl-3-butyldisiloxane with a boiling temperature of 166-169° C. Bottoms and separated-off hexamethyldisiloxane can be passed to further equilibrations.

Provenance & Evidence