Triethylamine → N-(4-nitrobenzyl)trifluoroacetoamide

HRID 856657

Reaktionsgleichung

Reaktionsgleichung von HRID 856657
Cl.[N+:2]([C:5]1[CH:12]=[CH:11][C:8]([CH2:9][NH2:10])=[CH:7][CH:6]=1)([O-:4])=[O:3].C(N(CC)CC)C.C([O:23][CH2:24][C:25]([F:28])([F:27])[F:26])(=O)C>C(#N)C>[N+:2]([C:5]1[CH:6]=[CH:7][C:8]([CH2:9][NH:10][C:24](=[O:23])[C:25]([F:28])([F:27])[F:26])=[CH:11][CH:12]=1)([O-:4])=[O:3]

Komponenten

5

Edukt 3

HCID 8471TriethylamineHCID 1362562,2,2-Trifluoroethyl AcetateHCID 112524674-Nitrobenzylamine hydrochloride

Produkt 1

HCID 14317262N-(4-nitrobenzyl)trifluoroacetoamide

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6342AcetonitrileLösungsmittel

Versuchsvorschrift

To a suspension of 4-nitrobenzylamine hydrochloride (10.0 g) and triethylamine (22.2 ml) in acetonitrile (100 ml) was added trifluoroethyl acetate (12.6 ml) at room temperature and the mixture was stirred for 24 hours. The solvent was removed under reduced pressure, water was added to the mixture and the mixture was extracted with ethyl acetate. The organic layer was washed with saturated brine, dried over magnesium sulfate and concentrated under reduced pressure. The precipitated crystals were collected by filtration. The crystals were washed with hexane, to give N-(4-nitrobenzyl)trifluoroacetoamide (12.79 g) as colorless crystals.

Aufarbeitung

  1. customThe solvent was removed under reduced pressure, water
  2. additionwas added to the mixture
  3. extractionthe mixture was extracted with ethyl acetate
  4. washThe organic layer was washed with saturated brine
  5. dry with materialdried over magnesium sulfate
  6. concentrationconcentrated under reduced pressure
  7. filtrationThe precipitated crystals were collected by filtration
  8. washThe crystals were washed with hexane

Quellen und Nachweise

ORD-Eintrag
ord-2b75692cde864675be581d7fbd123640
Quelldatensatz
uspto-grants-2007_08
Patentnummer
US07262185B2

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