N-bromobutanimide → 4-Bromo-3,5-difluoroaniline

HRID 1270728

Reaktionsgleichung

Reaktionsgleichung von HRID 1270728
[F:1][C:2]1[CH:3]=[C:4]([CH:6]=[C:7]([F:9])[CH:8]=1)[NH2:5].C1C(=O)N([Br:17])C(=O)C1>CN(C=O)C.CCOCC>[Br:17][C:8]1[C:2]([F:1])=[CH:3][C:4]([NH2:5])=[CH:6][C:7]=1[F:9]

Komponenten

5

Edukt 2

HCID 67184N-bromobutanimideHCID 965953,5-Difluoroaniline

Produkt 1

HCID 27362604-Bromo-3,5-difluoroaniline

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 3283Diethyl EtherLösungsmittelHCID 6228DimethylformamideLösungsmittel

Versuchsvorschrift

3,5-Difluoroaniline (10.0 g, 77.5 mmol) is dissolved in DMF (100 mL). NBS (13.9 g, 78.0 mmol) is added portionwise at room temperature. After stirring overnight at room temperature, the reaction mixture is diluted with Et2O and washed with brine. The separated organic phase is dried (Na2SO4) and concentrated to give an oil which is purified by column chromatography (methylene chloride/hexanes) to give 4-bromo-3,5-difluoroaniline.

Aufarbeitung

  1. washwashed with brine
  2. dry with materialThe separated organic phase is dried (Na2SO4)
  3. concentrationconcentrated
  4. customto give an oil which
  5. customis purified by column chromatography (methylene chloride/hexanes)

Quellen und Nachweise

ORD-Eintrag
ord-e552a0d6f13146c99cc37f51be6c777b
Quelldatensatz
uspto-grants-2007_04
Patentnummer
US07202364B2

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