Diethyl Ether → HCID 178506893, Verbindung

HRID 1256861Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1256861
[CH3:1][N:2](C)[C:3]1C(C)=CC=CC=1.C(OCC)C.[CH2:16]([Li:20])[CH2:17][CH2:18][CH3:19].[CH3:21][CH2:22][CH2:23]CCC>>[CH3:1][N:2]([CH:16]([Li:20])[C:17]1[CH:23]=[CH:22][CH:21]=[CH:19][CH:18]=1)[CH3:3]

Komponenten

5

Versuchsvorschrift

18 mL (0.12 mmol) of N,N-dimethyl-o-toluidine was placed in a 200 mL glass vessel, to which a mixed solvent of 50 mL of hexane and 16 mL of diethyl ether was added under a nitrogen atmosphere. 50 mL (2.6 mol/L) of a hexane solution of n-butyllithium was slowly added dropwise to the solution under stirring at room temperature over 25 minutes, and the solution was further stirred at room temperature for 45 hours. After completing the reaction, the precipitate was filtered off, and the resulting solid matter was rinsed with hexane and dried under reduced pressure at room temperature to provide 13 g of dimethylaminobenzyllithium (LiCH2C6H4N(CH3)2-o) (yield: 77%).

Aufarbeitung

  1. stirringthe solution was further stirred at room temperature for 45 hours
  2. customthe reaction
  3. filtrationthe precipitate was filtered off
  4. washthe resulting solid matter was rinsed with hexane
  5. customdried under reduced pressure at room temperature

Quellen und Nachweise

ORD-Eintrag
ord-0718aa2430c448d3ac584061527d9c73
Quelldatensatz
uspto-grants-2013_06
Patentnummer
US08461270B2

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