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HCID 4232364, Verbindung → 4,4-Dimethyl-4-silapentane-1-sulfonic acid

HRID 2184067
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 2184067
[CH3:1][Si:2]([CH3:11])([CH3:10])[CH2:3][CH2:4][CH2:5][S:6]([O-:9])(=[O:8])=[O:7].[Na+].C[Si](C)(C)CCCS([O-])(=O)=O>O>[CH3:10][Si:2]([CH3:1])([CH3:11])[CH2:3][CH2:4][CH2:5][S:6]([OH:9])(=[O:8])=[O:7]
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Komponenten

4

Edukt 2

HCID 4232364HCID 4232364, VerbindungHCID 5167273Sodium 3-(trimethylsilyl)-1-propanesulfonate

Produkt 1

HCID 748734,4-Dimethyl-4-silapentane-1-sulfonic acid

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

A solution of sodium 3-(trimethylsilyl)-1-propanesulfonate (13 grams, 59.5 mmol) dissolved in demineralized water (75 ml) was added dropwise into a short column packed with an excess (15-20 times the molar amount of 3-(trimethylsilyl)-1-propanesulfonate) of Tulsion T-42 MP(H+) acidic ion exchange resin. Then the resin bed was washed with water until the pH of the solution eluting from the column was about 5 to 6. The water solution of the free 3-(trimethylsilyl)-1-propanesulfonic acid thus obtained was neutralized with tetra-n-butylphosphonium hydroxide until the pH of the solution was about 5 to 5.5. The resulting mixture was extracted with chloroform (three times) and the combined chloroform washes was washed with water (three times). The chloroform layer was separated, dried with anhydrous sodium sulfate, and concentrated under reduced pressure to remove solvent and other volatiles. The residual material was finally dried at 40° C. and 0.1 mm Hg to afford tetra-n-butylphosphonium 3-(trimethylsilyl)-1-propanesulfonate as a white solid. The yield of the product was 26.9 grams, or 99% of the theoretical amount. Proton NMR spectrum of the compound indicated that it was the desired compound.

Aufarbeitung

  1. additionwas added dropwise into a short column
  2. washThen the resin bed was washed with water until the pH of the solution
  3. washeluting from the column

Quellen und Nachweise

ORD-Eintrag
ord-860e0977005e410f9cc2f89da84a6c4f
Quelldatensatz
uspto-grants-2005_05
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US06900257B2

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