HCID 22497279, compound → HCID 131724841, compound

HRID 1816076Notes

Reaction equation

HRID 1816076 reaction equation
[CH2:1]([O:4][CH2:5][CH2:6][O:7][CH:8]1[CH2:14][CH2:13][CH2:12][S:9]1(=[O:11])=[O:10])[CH:2]=[CH2:3].[CH3:15][Si:16]([CH3:26])([CH3:25])[O:17][CH:18]([SiH3:24])[O:19][Si:20]([CH3:23])([CH3:22])[CH3:21]>C1(C)C(C)=CC=CC=1>[CH3:21][Si:20]([CH3:23])([CH3:22])[O:19][CH:18]([SiH2:24][CH2:3][CH2:2][CH2:1][O:4][CH2:5][CH2:6][O:7][CH:8]1[CH2:14][CH2:13][CH2:12][S:9]1(=[O:10])=[O:11])[O:17][Si:16]([CH3:26])([CH3:25])[CH3:15]

Participants

4

Reactant 2

HCID 22497279HCID 22497279, compoundHCID 71317459HCID 71317459, compound2×

Product 1

HCID 131724841HCID 131724841, compoundYield 134.7%

Reagents, catalysts & solvents 1

HCID 7237O-XyleneSolvent

Procedure

A 500 ml three neck round bottom flask equipped with a magnetic stirrer, condenser, additional funnel, and pot thermometer was charged with 165.0 g (0.75 mol) of allyloxyethoxy sulfolane under appositive pressure of nitrogen. After heating to 80° C.-90° C., 61.2 g (0.28 mol) of bis(trimethylsiloxy)methylsilane was added, followed by 1 ml of Pt(0)-divinyltetramethyldisiloxane solution in xylene (2 wt % Pt). The pot temperature rose from 86° C. to approximately 102° C. The rest of 122.4 g (0.55 mol) of bis(trimethylsiloxy)methylsilane was added while maintaining a pot temperature of between 86° C.-106° C. The mixture was then maintained at a temperature between 86° C.-96° C. for 16 h and was distilled. 167.0 g (50.3%) pure bis(trimethylsiloxy)methylsilylpropoxyethoxy sulfolane was obtained. The pure product had a boiling point of 194° C.-200° C. at 0.4 mm Hg and a density of 1.412 at 25° C.

Workup

  1. temperatureAfter heating to 80° C.-90° C.
  2. customrose from 86° C. to approximately 102° C
  3. temperaturewhile maintaining a pot temperature of between 86° C.-106° C
  4. temperatureThe mixture was then maintained at a temperature between 86° C.-96° C. for 16 h
  5. distillationwas distilled

Sources & evidence

ORD record
ord-2563368170b34524a53dffb196aa4152
Source dataset
uspto-grants-2005_04
Patent number
US06881849B2

Reaction notes

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