Diisobutyl aluminium chloride → [8-(Dimethylamino)naphth-1-yl]diisobutylaluminium

HRID 898105

Reaktionsgleichung

Reaktionsgleichung von HRID 898105
[Cl-].[CH2:2]([Al+:6][CH2:7][CH:8]([CH3:10])[CH3:9])[CH:3]([CH3:5])[CH3:4].[CH3:11][N:12]([CH3:24])[C:13]1[CH:14]=[CH:15][CH:16]=[C:17]2[C:22]=1[C:21]([Li])=[CH:20][CH:19]=[CH:18]2>C(OCC)C>[CH3:11][N:12]([CH3:24])[C:13]1[CH:14]=[CH:15][CH:16]=[C:17]2[C:22]=1[C:21]([Al:6]([CH2:7][CH:8]([CH3:10])[CH3:9])[CH2:2][CH:3]([CH3:5])[CH3:4])=[CH:20][CH:19]=[CH:18]2

Komponenten

4

Edukt 2

HCID 16686353Diisobutyl aluminium chlorideHCID 178506672HCID 178506672, Verbindung

Produkt 1

HCID 72359367[8-(Dimethylamino)naphth-1-yl]diisobutylaluminiumAusbeute 70.907,102 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 3283Diethyl EtherLösungsmittel

Versuchsvorschrift

9.5 g (0.048 mmol) of diisobutylaluminium chloride were added dropwise to a suspension, cooled to −40° C., of 12.1 g (0.048 mmol) of [8-(dimethylamino)naphth-1-yl]lithium etherate and 100 ml of diethyl ether in an inert nitrogen atmosphere. After slow warming to room temperature, the mixture was stirred for a further 24 hours in order to complete the reaction. Filtration through a D4 frit and removal of the solvent by distillation gave 10.6 g of [8-(dimethylamino)naphth-1-yl]diisobutylaluminium (71%) as a colourless, oily liquid by fractional distillation from the residue.

Aufarbeitung

  1. customthe reaction
  2. filtrationFiltration
  3. customthrough a D4 frit and removal of the solvent
  4. distillationby distillation

Quellen und Nachweise

ORD-Eintrag
ord-57bb6f8ddb4c451aaa3533668a37e62f
Quelldatensatz
uspto-grants-2008_04
Patentnummer
US07351678B2

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