Potassium Hydroxide → HCID 86712060, compound

HRID 1852312Notes

Reaction equation

HRID 1852312 reaction equation
[CH2:1]([Si:9]([O:14][CH3:15])([O:12][CH3:13])[O:10][CH3:11])[CH2:2][CH2:3][CH2:4][CH2:5][CH:6]([CH3:8])[CH3:7].CC(CC(C)(C)C)C[Si](OC)(OC)[O:20]C.[OH-].[K+:32]>O>[CH2:1]([Si:9]([O:14][CH3:15])([O:10][CH3:11])[O:12][CH3:13])[CH2:2][CH2:3][CH2:4][CH2:5][CH:6]([CH3:8])[CH3:7].[OH-:20].[K+:32]

Participants

5

Reactant 3

HCID 14797Potassium HydroxideHCID 118163Trimethoxy(2,4,4-trimethylpentyl)silaneHCID 17780421HCID 17780421, compound

Product 1

HCID 86712060HCID 86712060, compound

Reagents, catalysts & solvents 1

HCID 962WaterSolvent3×

Procedure

A 500 ml 5-neck round-bottom flask rendered inert with nitrogen and equipped with paddle stirrer, dropping funnel, thermometer, and water separator with reflux condenser is charged with 60 g (0.25 mol) of isooctyltrimethoxysilane (=2,4,4-trimethyl-1-pentyltrimethoxysilane, available commercially from Wacker Chemie AG as SILRES® BS 1316), and 55.7 g of Isopar E (isoparaffinic hydrocarbon mixture with a boiling range of 113-143° C., available commercially from ExxonMobil). With stirring 27.8 g of 43% strength potassium hydroxide solution (0.21 mol KOH) are metered in over 6 minutes. This is followed by heating to reflux, with the water separator filled to the brim with Isopar E. The distillate separates out as the lower phase in the water separator. Up to a boiling temperature of 119° C., 33.5 g of clear colorless distillate are collected, which according to analysis by gas chromatography contains 64.6% methanol and 34.7% water. Therefore 90% of the methoxy radicals are hydrolyzed. During the distillation, the reaction mixture undergoes transformation into a suspension. The volatile constituents are removed by distillation at 100° C./4 hPa. The residue left is 53.3 g of a white, fine powder whose solids content is 99.8% (determined using the HR73 Halogen Moisture Analyzer solids content balance from Mettler Toledo at 160° C.)

Workup

  1. customA 500 ml 5-neck round-bottom flask rendered inert with nitrogen
  2. customequipped with paddle stirrer
  3. temperaturewith reflux condenser
  4. customare metered in over 6 minutes
  5. temperatureby heating
  6. additionseparator filled to the brim with Isopar E
  7. distillationUp to a boiling temperature of 119° C., 33.5 g of clear colorless distillate are collected
  8. distillationDuring the distillation
  9. customThe volatile constituents are removed by distillation at 100° C./4 hPa
  10. waitThe residue left
  11. customat 160° C.

Sources & evidence

ORD record
ord-419bdf70865d4d4faf772608dbd72d88
Source dataset
uspto-grants-2015_02
Patent number
US08961672B2

Reaction notes

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