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Sodium Methoxide → 2,2',4'-Trifluoro-3-methoxybiphenyl-4-carbaldehyde

HRID 2272498
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Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 2272498
[CH3:1][O-:2].[Na+].[F:4][C:5]1[C:10](F)=[C:9]([CH:12]=[O:13])[CH:8]=[CH:7][C:6]=1[C:14]1[CH:19]=[CH:18][C:17]([F:20])=[CH:16][C:15]=1[F:21]>CO>[F:4][C:5]1[C:10]([O:2][CH3:1])=[C:9]([CH:12]=[O:13])[CH:8]=[CH:7][C:6]=1[C:14]1[CH:19]=[CH:18][C:17]([F:20])=[CH:16][C:15]=1[F:21]
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Komponenten

4

Edukt 2

HCID 10942334Sodium MethoxideHCID 1179922312,2',3,4'-Tetrafluoro-[1,1'-biphenyl]-4-carbaldehyde

Produkt 1

HCID 1179920892,2',4'-Trifluoro-3-methoxybiphenyl-4-carbaldehydeAusbeute 99,1 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel

Versuchsvorschrift

Sodium methoxide (28% methanol solution, 5.64 g) was added at room temperature to a methanol (120 mL) solution of 2,2′,3,4′-tetrafluorobiphenyl-4-carbaldehyde (4.95 g), and the mixture was heated to reflux for 16 hours in a nitrogen atmosphere. Then, the solvent was distilled off under reduced pressure. The residue was diluted with ethyl acetate and water, followed by extraction with ethyl acetate. The organic layer was separated, washed with water and saturated saline in this order, and dried over anhydrous magnesium sulfate, and then, the solvent was distilled off under reduced pressure to obtain the title compound (5.14 g).

Aufarbeitung

  1. temperaturethe mixture was heated
  2. temperatureto reflux for 16 hours in a nitrogen atmosphere
  3. distillationThen, the solvent was distilled off under reduced pressure
  4. additionThe residue was diluted with ethyl acetate and water
  5. extractionfollowed by extraction with ethyl acetate
  6. customThe organic layer was separated
  7. washwashed with water and saturated saline in this order
  8. dry with materialdried over anhydrous magnesium sulfate
  9. distillationthe solvent was distilled off under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-ea26e10fd608429a9e1a59ade20c20ec
Quelldatensatz
uspto-grants-2015_09
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US09120777B2

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