Water → 7,8-difluoro-4-methyl-3,4-dihydro-1,4-benzoxazepin-5(2H)-one

HRID 548707

Reaktionsgleichung

Reaktionsgleichung von HRID 548707
[H-].[Na+].F[C:4]1[CH:16]=[C:15]([F:17])[C:14]([F:18])=[CH:13][C:5]=1[C:6]([N:8]([CH2:10][CH2:11][OH:12])[CH3:9])=[O:7].O>CN(C=O)C>[F:18][C:14]1[C:15]([F:17])=[CH:16][C:4]2[O:12][CH2:11][CH2:10][N:8]([CH3:9])[C:6](=[O:7])[C:5]=2[CH:13]=1

Komponenten

5

Edukt 3

HCID 962WaterHCID 24758Sodium hydrideHCID 576631992,4,5-trifluoro-N-(2-hydroxyethyl)-N-methylbenzamide

Produkt 1

HCID 576632107,8-difluoro-4-methyl-3,4-dihydro-1,4-benzoxazepin-5(2H)-oneAusbeute 100 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel

Versuchsvorschrift

Sodium hydride (52 mg, 1.29 mmol) was added portionwise to a solution of 2,4,5-trifluoro-N-(2-hydroxyethyl)-N-methylbenzamide (300 mg, 1.29 mmol) in DMF (13 mL) and reaction was allowed to stir at RT for 2 hours. Water (30 mL) was added and the white solution was extracted with ethyl acetate (3×30 mL) and dried (MgSO4), filtered and evaporated to give the desired compound as a colourless oil (275 mg). The compound was used without further purification.

Aufarbeitung

  1. extractionthe white solution was extracted with ethyl acetate (3×30 mL)
  2. dry with materialdried (MgSO4)
  3. filtrationfiltered
  4. customevaporated

Quellen und Nachweise

ORD-Eintrag
ord-45000c9431a148b18dca0445a3e19d5a
Quelldatensatz
uspto-grants-2011_05
Patentnummer
US07943607B2

Verknüpfte Notizen

Wird geladen…