Chlorotrimethylsilane → 1-Trimethylsiloxyindene

HRID 34263

Reaktionsgleichung

Reaktionsgleichung von HRID 34263
[CH3:1][Si:2](Cl)([CH3:4])[CH3:3].C(N(CC)CC)C.[C:13]1(=[O:22])[C:21]2[C:16](=[CH:17][CH:18]=[CH:19][CH:20]=2)[CH2:15][CH2:14]1>CN(C)C=O.CCCCC>[CH3:1][Si:2]([CH3:4])([CH3:3])[O:22][CH:13]1[C:21]2[C:16](=[CH:17][CH:18]=[CH:19][CH:20]=2)[CH:15]=[CH:14]1

Komponenten

6

Edukt 3

HCID 6397ChlorotrimethylsilaneHCID 67351-IndanoneHCID 8471Triethylamine

Produkt 1

HCID 140001951-Trimethylsiloxyindene

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 6228DimethylformamideLösungsmittelHCID 8003PentaneLösungsmittel

Versuchsvorschrift

Trimethylsilyl chloride (5.7 g, 52.3 mmole), triethylamine (11.71 g, 116 mmole), and 1-indanone (6.22 g, 47.1 mmole) were dissolved in dimethyl formamide (25 mL) and refluxed for 17 hours. After cooling, the mixture was diluted with pentane (50 mL) and washed four times with saturated sodium bicarbonate. After backwashing the aqueous phase with pentane the organic layers were combined, washed with cold 2N HCl and cold saturated sodium bicarbonate, then dried over MgSO4. The solvent was evaporated and the residue distilled (bp 123°-125° C.).

Aufarbeitung

  1. temperaturerefluxed for 17 hours
  2. temperatureAfter cooling
  3. washwashed four times with saturated sodium bicarbonate
  4. washwashed with cold 2N HCl and cold saturated sodium bicarbonate
  5. dry with materialdried over MgSO4
  6. customThe solvent was evaporated
  7. distillationthe residue distilled (bp 123°-125° C.)

Quellen und Nachweise

ORD-Eintrag
ord-4d1857117c354952a4bf1552ec242980
Quelldatensatz
uspto-grants-1988_08
Patentnummer
US04761403

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