Triethylamine → HCID 137328355, Verbindung

HRID 1092372Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1092372
[Br:1][C:2]1[CH:3]=[C:4]([OH:8])[CH:5]=[CH:6][CH:7]=1.CCN(CC)CC.[CH3:16][Si:17](Cl)([CH3:20])[CH2:18][CH3:19]>C1COCC1>[Br:1][C:2]1[CH:3]=[C:4]([CH:5]=[CH:6][CH:7]=1)[O:8][CH2:19][CH2:18][SiH:17]([CH3:20])[CH3:16]

Komponenten

5

Edukt 3

HCID 8471TriethylamineHCID 115633-BromophenolHCID 138863Ethyldimethylchlorosilane

Produkt 1

HCID 137328355HCID 137328355, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel

Reaktionsbedingungen

Temperatur
0 °C

Versuchsvorschrift

To a stirred solution of 3-bromophenol (0.60 g, 3.47 mmol) in dry THF (15 mL) under nitrogen was added Et3N (0.48 mL, 3.47 mmol). A clear yellow solution formed immediately; after cooling to 0° C., dimethylethylsilyl chloride (0.43 g, 0.49 mL, 3.47 mmol) was added by syringe over a period of 10 minutes. The yellow color disappeared in 10 min, and a white cloudy solution formed. After 3 hr the thick reaction mixture was filtered, washed with 15 mL of hexane, and filtered again. Concentration gave a clear oil (quantitative weight recovery) that was used in the next step without any purification.

Aufarbeitung

  1. customA clear yellow solution formed immediately
  2. customa white cloudy solution formed
  3. filtrationAfter 3 hr the thick reaction mixture was filtered
  4. washwashed with 15 mL of hexane
  5. filtrationfiltered again
  6. concentrationConcentration
  7. customgave a clear oil (quantitative weight recovery) that
  8. customwas used in the next step without any purification

Quellen und Nachweise

ORD-Eintrag
ord-09688436a97d4243bc8e302032c81875
Quelldatensatz
uspto-grants-2012_03
Patentnummer
US08129428B2

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