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Dimethylformamide → HCID 58386652, Verbindung

HRID 74541
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 74541
C(N1[C:12]2[C:7](=[C:8]([F:14])[C:9]([F:13])=[CH:10][CH:11]=2)[CH2:6]C1=O)(=O)C.[H-].[Na+].I[CH3:19].[CH3:20][N:21]([CH:23]=[O:24])C>>[F:13][C:9]1[C:8]([F:14])=[CH:7][CH:6]=[C:20]2[C:10]=1[C:11]([CH3:12])([CH3:19])[C:23](=[O:24])[NH:21]2
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 4

HCID 6228DimethylformamideHCID 6328Methyl iodideHCID 24758Sodium hydrideHCID 58386747HCID 58386747, Verbindung

Produkt 1

HCID 58386652HCID 58386652, Verbindung

Versuchsvorschrift

0.50 g (2.4 mmol) 1-acetyl-4,5-difluoro-1,3-dihydro-indol-2-one were placed in 10 mL DMF under argon. 0.22 g (5.1 mmol) sodium hydride (55%) were added at 0° C. and the reaction mixture was stirred for 1 h. Then 0.32 mL (5.1 mmol) iodomethane were added dropwise. The reaction mixture was stirred overnight at RT, poured onto water and extracted with EtOAc. The organic phase was dried, filtered and concentrated to dryness by rotary evaporation. The residue was purified by HPLC. The product-containing fractions were combined and concentrated to dryness by rotary evaporation.

Aufarbeitung

  1. stirringThe reaction mixture was stirred overnight at RT
  2. additionpoured onto water
  3. extractionextracted with EtOAc
  4. customThe organic phase was dried
  5. filtrationfiltered
  6. concentrationconcentrated to dryness by rotary evaporation
  7. customThe residue was purified by HPLC
  8. concentrationconcentrated to dryness by rotary evaporation

Quellen und Nachweise

ORD-Eintrag
ord-0e4565496f7944c39d13adfff8d6afd9
Quelldatensatz
uspto-grants-2014_09
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08829006B2

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