Acetic Acid → Diisopropylether methanol

HRID 893343

Reaktionsgleichung

Reaktionsgleichung von HRID 893343
CC1C=C2[C:8](=[CH:9][CH:10]=1)N[C:6](=[O:11])C2.[CH3:12][C:13]([O-:15])=O.[Na+].[C:17](O)(=O)C>>[CH3:6][OH:11].[O:15]([CH:9]([CH3:8])[CH3:10])[CH:13]([CH3:12])[CH3:17]

Komponenten

4

Edukt 3

HCID 176Acetic AcidHCID 517045Sodium AcetateHCID 53257165-Methylindolin-2-one

Produkt 1

HCID 21882575Diisopropylether methanol

Versuchsvorschrift

A mixture of 5-methyl-2-oxindole (2.94 g, 0.02 mol), 3,5-di-tertiary-butyl-4-hydroxybenzoldehyde (4.68 g, 0.02 mol), and anyydrous NaOAc (5.75 g, 0.07 mol) in glacial acetic acid (100 mL) was heated to reflux for 18 hours. The cooled reaction mixture was poured into ice-water mixture when a yellow product precipitated out. It was recrystallized from CH2Cl2 --CH3OH-iso-Pr2O to give the analytical sample. Yield 2.16 g (28.7%), mp 230°-234° C.

Aufarbeitung

  1. temperaturewas heated
  2. temperatureto reflux for 18 hours
  3. customThe cooled reaction mixture
  4. customprecipitated out
  5. customIt was recrystallized from CH2Cl2

Quellen und Nachweise

ORD-Eintrag
ord-9e9feb137dcb4903abe56920c948ff41
Quelldatensatz
uspto-grants-1992_06
Patentnummer
US05124347

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