Sodium sulfate decahydrate → 3-(3,4,5-Trimethoxyphenyl)Propan-1-Ol

HRID 1109657Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1109657
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH2:13][CH2:14][C:15](OC)=[O:16])[CH:6]=[C:7]([O:11][CH3:12])[C:8]=1[O:9][CH3:10].[H-].[Al+3].[Li+].[H-].[H-].[H-].O.O.O.O.O.O.O.O.O.O.S([O-])([O-])(=O)=O.[Na+].[Na+]>O1CCCC1>[CH3:12][O:11][C:7]1[CH:6]=[C:5]([CH2:13][CH2:14][CH2:15][OH:16])[CH:4]=[C:3]([O:2][CH3:1])[C:8]=1[O:9][CH3:10]

Komponenten

5

Edukt 3

HCID 62649Sodium sulfate decahydrateHCID 2797678Methyl 3-(3,4,5-trimethoxyphenyl)propanoateHCID 21226445Aluminium lithium hydride

Produkt 1

HCID 64288433-(3,4,5-Trimethoxyphenyl)Propan-1-OlAusbeute 97,6 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel2×

Reaktionsbedingungen

Temperatur
0 °C

Versuchsvorschrift

A solution of methyl 3-(3,4,5-trimethoxyphenyl)propanoate (11.03 g, 0.043 mol) in tetrahydrofuran (20 ml) was added dropwise to a suspension of lithium aluminum hydride (1.6 g, 0.042 mol) in 20 ml of tetrahydrofuran, said suspension having been cooled to 0° C., followed by stirring at room temperature for 19 hours. After the addition of sodium sulfate decahydrate, the resulting mixture was stirred further at room temperature for one hour. Insoluble matter was removed by filtration and the filtrate was concentrated, whereby 9.5 g of the title compound were obtained as colorless oil (yield: 96.8%).

Aufarbeitung

  1. stirringthe resulting mixture was stirred further at room temperature for one hour
  2. customInsoluble matter was removed by filtration
  3. concentrationthe filtrate was concentrated

Quellen und Nachweise

ORD-Eintrag
ord-4e7fd868d91048dbbb82401081de07de
Quelldatensatz
uspto-grants-1994_06
Patentnummer
US05321135

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