Water → HCID 22327806, Verbindung

HRID 271003Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 271003
[CH3:1][C:2]([CH2:8][CH:9]([CH3:11])[CH3:10])=[C:3]1[CH:7]=[CH:6][CH:5]=[CH:4]1.[CH3:12][Li].O>CCOCC>[CH3:1][C:2]([C:3]1[CH2:7][CH:6]=[CH:5][CH:4]=1)([CH3:12])[CH2:8][CH:9]([CH3:11])[CH3:10]

Komponenten

5

Edukt 3

HCID 962WaterHCID 5626186-Methyl-6-isobutylfulveneHCID 178418348HCID 178418348, Verbindung

Produkt 1

HCID 22327806HCID 22327806, VerbindungAusbeute 80 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 3283Diethyl EtherLösungsmittel2×

Versuchsvorschrift

To a solution of 8.00 g (54.0 mmol) of 6-methyl-6-isobutylfulvene in 30 ml of ether, 54.0 ml (61.6 mmol) of an ether solution of methyllithium was dropwise added in a nitrogen atmosphere with ice cooling, followed by stirring at room temperature for 4 days. Then, 30 ml of water was added. The separated organic phase was washed with water and a saturated saline solution, then dried over magnesium sulfate and filtered. From the filtrate, the solvent was removed under reduced pressure to obtain a liquid. The liquid was subjected to vacuum distillation (120° C./25 mmHg) to obtain 7.10 g (43.2 mmol) of a light yellow liquid (yield: 80%)

Aufarbeitung

  1. washThe separated organic phase was washed with water
  2. dry with materiala saturated saline solution, then dried over magnesium sulfate
  3. filtrationfiltered
  4. customFrom the filtrate, the solvent was removed under reduced pressure
  5. customto obtain a liquid
  6. distillationThe liquid was subjected to vacuum distillation (120° C./25 mmHg)

Quellen und Nachweise

ORD-Eintrag
ord-911eee3c27904bc59bc847f14493b0c2
Quelldatensatz
uspto-grants-2008_11
Patentnummer
US07449533B2

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