Potassium Hydroxide → HCID 86712058, compound

HRID 1852310Notes

Reaction equation

HRID 1852310 reaction equation
[CH2:1]([Si:7]([O:12][CH3:13])([O:10][CH3:11])[O:8][CH3:9])[CH2:2][CH2:3][CH:4]([CH3:6])[CH3:5].[OH-:14].[K+:15]>O>[CH2:1]([Si:7]([O:12][CH3:13])([O:8][CH3:9])[O:10][CH3:11])[CH2:2][CH2:3][CH:4]([CH3:5])[CH3:6].[OH-:14].[K+:15]

Participants

4

Reactant 2

HCID 14797Potassium HydroxideHCID 3038541Trimethoxy(4-methylpentyl)silane

Product 1

HCID 86712058HCID 86712058, compound

Reagents, catalysts & solvents 1

HCID 962WaterSolvent2×

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 27 g (0.13 mol) of isohexyltrimethoxysilane (=4-methyl-1-pentyltrimethoxysilane laboratory product, prepared by reaction of isohexyltrichlorosilane with methanol; isohexyltrichlorosilane is available through hydrosilylation reaction from 4-methyl-1-pentene and trichlorosilane), and 25 g of Isopar E (isoparaffinic hydrocarbon mixture with a boiling range of 113-143° C., available commercially from ExxonMobil). With stirring at 300 rpm, 14.7 g of 50% strength potassium hydroxide solution (0.13 mol KOH) are metered in over 10 minutes, during which the solution is heated to reflux. The distillate separates out as the lower phase in the water separator. Up to a boiling temperature of 118° C., 16 g of clear colorless distillate are collected, which according to analysis by gas chromatography contains 77.1% methanol, 22.1% water, and 0.7% Isopar E. The hydrolysis of the methoxy radicals, accordingly, is quantitative. During the distillation, the reaction mixture undergoes transformation into a suspension. The volatile constituents are removed by distillation at 70° C./4 hPa. The residue left is a white, floury powder whose solids content is 99.4% (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 10 minutes, during which
  5. temperatureis heated to reflux
  6. distillationUp to a boiling temperature of 118° C., 16 g of clear colorless distillate are collected
  7. customThe hydrolysis of the methoxy radicals
  8. distillationDuring the distillation
  9. customThe volatile constituents are removed by distillation at 70° C./4 hPa
  10. waitThe residue left
  11. customat 160° C.

Sources & evidence

ORD record
ord-3974496276fe48158fe8b5af8f5e63d1
Source dataset
uspto-grants-2015_02
Patent number
US08961672B2

Reaction notes

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