3-Hydroxybenzaldehyde → HCID 21071449, Verbindung

HRID 1371954Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1371954
[F:1][C:2]([F:19])([CH:16]([F:18])[F:17])[CH2:3][O:4][C:5]1[CH:6]=[C:7]([CH:12]=[CH:13][C:14]=1C)S([O-])(=O)=O.[OH:20][C:21]1C=C(C=CC=1)C=O.C(=O)([O-])[O-].[K+].[K+]>CN(C)C=O>[F:19][C:2]([F:1])([CH:16]([F:17])[F:18])[CH2:3][O:4][C:5]1[CH:6]=[C:7]([CH:12]=[CH:13][CH:14]=1)[CH:21]=[O:20]

Komponenten

5

Edukt 3

HCID 1013-HydroxybenzaldehydeHCID 11430Potassium CarbonateHCID 21071450HCID 21071450, Verbindung

Produkt 1

HCID 21071449HCID 21071449, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel

Reaktionsbedingungen

Temperatur
20 °C

Versuchsvorschrift

Combine 3-(2,2,3,3-tetrafluoropropoxy)tosylate (5.72 g, 17.2 mmol), 3-hydroxybenzaldehyde (2.44 g, 20.0 mmol), dimethylformamide (36 ml) and powdered potassium carbonate (3.03 g) and heat at 110° C. for 10 h. Cool to 20° C. Pass through a bed of aluminium-oxide-90 (57.2 g, 70–230 mesh, grade II–III, Brockmann: Merck # 1.01097) and elute with toluene (120 ml). Wash the eluted organic phase with 1N HCl (36 ml) and then water. Evaporate the organic layer under reduced pressure to give the title compound.

Aufarbeitung

  1. washPass through a bed of aluminium-oxide-90 (57.2 g, 70–230 mesh, grade II–III, Brockmann: Merck # 1.01097) and elute with toluene (120 ml)
  2. washWash the eluted organic phase with 1N HCl (36 ml)
  3. customEvaporate the organic layer under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-d20678c3df594e1597028407b2f52ed1
Quelldatensatz
uspto-grants-2007_01
Patentnummer
US07157488B2

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