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Dimethylformamide → 5,6-Difluoro-1-indanone

HRID 2247603
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Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 2247603
C(Cl)(=O)C(Cl)=O.CN(C=O)C.[F:12][C:13]1[CH:14]=[C:15]([CH:21]=[CH:22][C:23]=1[F:24])[CH2:16][CH2:17][C:18]([OH:20])=O>ClCCl>[F:12][C:13]1[CH:14]=[C:15]2[C:21](=[CH:22][C:23]=1[F:24])[C:18](=[O:20])[CH2:17][CH2:16]2
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 3

HCID 6228DimethylformamideHCID 65578Oxalyl chlorideHCID 27789943,4-Difluorohydrocinnamic acid

Produkt 1

HCID 117689445,6-Difluoro-1-indanoneAusbeute 29,6 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

Oxalyl chloride (1.12 mL) and DMF (78.2 mg) were added to a solution of 3,4-difluorohydrocinnamic acid (2.00 g) in dichloromethane (3.0 mL) at 0° C., and the reaction solution was stirred at room temperature overnight. After confirming that the raw materials disappeared, the reaction solution was concentrated under reduced pressure. Next, a solution of the resulting residue in dichloromethane (10 mL) was added to a solution of aluminum chloride (2.13 g) in dichloromethane (20 mL) at −30° C. The reaction solution was stirred at room temperature for 1.5 hours. After confirming that the raw materials disappeared, the reaction solution was poured into ice water. The solution was extracted with ethyl acetate. The organic layer was washed with brine, and then dried over anhydrous magnesium sulfate and concentrated under reduced pressure. The resulting residue was purified by silica gel chromatography (elution solvent: heptane-ethyl acetate system) to obtain 535 mg of the title compound. The physical properties of the compound are as follows.

Aufarbeitung

  1. concentrationthe reaction solution was concentrated under reduced pressure
  2. additionNext, a solution of the resulting residue in dichloromethane (10 mL) was added to a solution of aluminum chloride (2.13 g) in dichloromethane (20 mL) at −30° C
  3. stirringThe reaction solution was stirred at room temperature for 1.5 hours
  4. additionthe reaction solution was poured into ice water
  5. extractionThe solution was extracted with ethyl acetate
  6. washThe organic layer was washed with brine
  7. dry with materialdried over anhydrous magnesium sulfate
  8. concentrationconcentrated under reduced pressure
  9. customThe resulting residue was purified by silica gel chromatography (elution solvent: heptane-ethyl acetate system)

Quellen und Nachweise

ORD-Eintrag
ord-bca7088e4dfe4e09b4779085f80b9666
Quelldatensatz
uspto-grants-2010_03
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US07687640B2

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