Aluminium lithium hydride → HCID 66959407, Verbindung

HRID 1958861Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1958861
[CH3:1][C:2]1[CH:19]=[CH:18][CH:17]=[C:16]([CH3:20])[C:3]=1[CH2:4][O:5][C:6]1[C:7]([O:14][CH3:15])=[C:8]([CH:11]=[CH:12][CH:13]=1)[CH:9]=[O:10].[H-].[H-].[H-].[H-].[Li+].[Al+3]>C1COCC1>[CH3:1][C:2]1[CH:19]=[CH:18][CH:17]=[C:16]([CH3:20])[C:3]=1[CH2:4][O:5][C:6]1[C:7]([O:14][CH3:15])=[C:8]([CH2:9][OH:10])[CH:11]=[CH:12][CH:13]=1

Komponenten

4

Edukt 2

HCID 21226445Aluminium lithium hydrideHCID 866570083-(2,6-Dimethylbenzyloxy)-2-methoxybenzaldehyde

Produkt 1

HCID 66959407HCID 66959407, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel

Versuchsvorschrift

To a solution of 3-(2,6-Dimethylbenzyloxy)-2-methoxybenzaldehyde (Step B, 10.6 g, 32.7 mmol) in dry THF (40 ml) was added drop wise LiAlH4 (1M in THF, 0.95 g, 23.7 mmol) at 0° C. under argon. The reaction mixture was stirred for 1 hours or until all the starting material is consumed, then quenched by adding water slowly, followed by addition of 1N HCl (5 ml), water (10 ml), and EtOAc (20 ml) was added to the reaction mixture. The reaction mixture was concentrated, and passed through a short silica gel column using ethyl acetate to give the title compound as an off white solid.

Aufarbeitung

  1. customis consumed
  2. customquenched
  3. additionby adding water slowly
  4. additionfollowed by addition of 1N HCl (5 ml), water (10 ml), and EtOAc (20 ml)
  5. additionwas added to the reaction mixture
  6. concentrationThe reaction mixture was concentrated

Quellen und Nachweise

ORD-Eintrag
ord-f117fc55acda429b91553d365c579183
Quelldatensatz
uspto-grants-2013_04
Patentnummer
US08410154B2

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