Ammonia → HCID 17978705, compound

HRID 2223006Notes

Reaction equation

HRID 2223006 reaction equation
[CH3:1][Si:2]([CH3:9])([CH3:8])[O:3][Si:4]([CH3:7])([CH3:6])[CH3:5].F[C:11](F)(S(O)(=O)=O)[C:12](F)(F)[C:13](F)(F)C(F)(F)F.N>O>[CH3:1][Si:2]([CH3:9])([CH3:8])[O:3][Si:4]([CH3:7])([CH3:6])[CH2:5][CH2:11][CH2:12][CH3:13]

Participants

5

Reactant 3

HCID 222AmmoniaHCID 24764HexamethyldisiloxaneHCID 67815Perfluorobutanesulfonic acid

Product 1

HCID 17978705HCID 17978705, compound

Reagents, catalysts & solvents 1

HCID 962WaterSolvent2×

Procedure

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.

Workup

  1. customequipped with stirrer
  2. distillationdistilled to 110° C.
  3. temperaturecooled
  4. filtrationfiltered
  5. customas result of fractional distillation

Sources & evidence

ORD record
ord-aff711b7f979456c965947adf95617cb
Source dataset
uspto-grants-2008_05
Patent number
US07374771B2

Reaction notes

Loading…