Potassium Hydroxide → HCID 86748951, compound

HRID 2399177Notes

Reaction equation

HRID 2399177 reaction equation
[CH3:1][Si:2]1([O:11]C)[CH:7]=[CH:6][Si:5]([CH3:10])(OC)[CH:4]=[CH:3]1.[OH-:13].[K+:14].[SiH4]>CO.O>[CH3:1][Si:2]1[CH2:7][CH2:6][Si:5]([CH3:10])=[CH:4][CH:3]=1.[SiH:2]([O-:11])=[O:13].[K+:14]

Participants

6

Reactant 3

HCID 14797Potassium Hydroxide2×HCID 23953SilaneHCID 54204799HCID 54204799, compound

Product 2

HCID 86748951HCID 86748951, compoundHCID 131719116HCID 131719116, compound

Reagents, catalysts & solvents 1

HCID 22242641Methanol--water (1/1)Solvent

Procedure

The impure sym-1,4-dimethyl-1,4-dimethoxy-1,4-disilacyclohexadiene is next reacted with potassium hydroxide dissolved in a methanol/water solution by slowly adding the silane to the KOH solution. The solution is then filtered and vacuum dried to remove most of the solvent. Tetrahydrofuran is then added, causing a precipitate to form. The precipitate is next filtered and washed with tetrahydrofuran and ether, and then recrystallized from isopropanol. A final wash of the solids with isopropanol and pentane gives pure 1,4-dimethyl- 1,4-disilacyclohexadiene- 1,4-di (potassium silanoate ). The 1,4-dimethyl-1,4-disilacyclohexadiene-,4-di(potassium silanoate) is next dissolved in ethanol. Concentrated hydrochloric acid is added to the solution, causing potassium chloride to precipitate out. Water and methylene chloride are then added to the solution, dissolving the potassium chloride and forming a two phase mixture. The organic phase is then decanted from the mixture. Upon evaporation of the methylene chloride at ambient temperature, an elastomer results. This elastomer is the new compound poly-1,4-oxo1,4-dimethyl- 1,4-disilacyclohexadiene.

Workup

  1. filtrationThe solution is then filtered
  2. customvacuum dried
  3. customto remove most of the solvent
  4. additionTetrahydrofuran is then added
  5. customto form
  6. filtrationThe precipitate is next filtered
  7. washwashed with tetrahydrofuran and ether
  8. customrecrystallized from isopropanol
  9. washA final wash of the solids with isopropanol and pentane

Sources & evidence

ORD record
ord-edf549728bbd4b5c845a7ba792b13d6b
Source dataset
uspto-grants-1995_09
Patent number
USH0001486

Reaction notes

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