Methanol → HCID 23249620, Verbindung

HRID 658961Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 658961
[O:1]([CH2:9][CH2:10][CH2:11][CH2:12]/[CH:13]=[C:14](\[CH3:20])/[C:15](OCC)=[O:16])[Si:2]([C:5]([CH3:8])([CH3:7])[CH3:6])([CH3:4])[CH3:3].[H-].C([Al+]CC(C)C)C(C)C.CCCCCC.CO.O.O.O.O.O.O.O.O.O.O.S([O-])([O-])(=O)=O.[Na+].[Na+]>C(Cl)Cl>[O:1]([CH2:9][CH2:10][CH2:11][CH2:12]/[CH:13]=[C:14](\[CH3:20])/[CH2:15][OH:16])[Si:2]([C:5]([CH3:7])([CH3:8])[CH3:6])([CH3:4])[CH3:3]

Komponenten

6

Edukt 4

HCID 887MethanolHCID 62649Sodium sulfate decahydrateHCID 11055704(E)-ethyl 7-(tert-butyldimethylsiloxy)-2-methyl-2-heptenateHCID 21273587HCID 21273587, Verbindung

Produkt 1

HCID 23249620HCID 23249620, VerbindungAusbeute 100 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

To a methylene chloride solution (200 ml) of Ester 4 (15.84 g; 0.0528 mol), a 0.95 M diisobutylaluminiumhydride-hexane solution (139 ml; 0.132 mol) is added at 0° C. and the whole is stirred for 1 hour. After stirring, methanol (7 ml; 0.160 mol) and sodium sulfate decahydrate (68.0 g; 0.211 mol) are added thereto and the whole is stirred at room temperature for 30 min. Sodiumsulfatedecahydrate is filtered using Chloroform (21), and the solvent is distilled off under reduced pressure to produce Alcohol 5 (13.60 g; 0.0528 mol) of 100% in yield.

Aufarbeitung

  1. stirringAfter stirring
  2. stirringthe whole is stirred at room temperature for 30 min
  3. filtrationSodiumsulfatedecahydrate is filtered
  4. distillationthe solvent is distilled off under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-40b47e8a91e14055884f7acca915c8ef
Quelldatensatz
uspto-grants-2011_12
Patentnummer
USRE043038E1

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