Tetrahydrofuran → HCID 178449877, Verbindung

HRID 570746Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 570746
[F:1][C:2]([F:13])([F:12])[CH2:3][O:4][C:5]1[CH:11]=[CH:10][C:8]([NH2:9])=[CH:7][CH:6]=1.C([N:16]([CH2:19][CH3:20])CC)C.[CH2:21]1COC[CH2:22]1.C(OCC)(=O)C>O>[F:1][C:2]([F:12])([F:13])[CH2:3][O:4][C:5]1[CH:11]=[CH:10][C:8]([NH:9][C:19](=[NH:16])[CH2:20][CH2:21][CH3:22])=[CH:7][CH:6]=1

Komponenten

6

Edukt 4

HCID 8028TetrahydrofuranHCID 8471TriethylamineHCID 8857Ethyl AcetateHCID 27771194-(2,2,2-Trifluoroethoxy)aniline

Produkt 1

HCID 178449877HCID 178449877, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Reaktionsbedingungen

Temperatur
70 °C

Versuchsvorschrift

A mixture of ethyl butylimidate hydrochloride (10.0 g), 4-(2,2,2-trifluoroethoxy)aniline (12.6 g), triethylamine (6.67 g) and THF (250 mL) was stirred at 70° C. for 2 days. To the reaction mixture were added ethyl acetate and water, and the mixture was extracted with ethyl acetate. The extract was washed with saturated brine, dried over magnesium sulfate, and concentrated under reduced pressure. The residue was subjected to aminopropylsilane-bonded silica gel column chromatography (ethyl acetate/hexane) to give the title compound (4.80 g) as a solid.

Aufarbeitung

  1. extractionthe mixture was extracted with ethyl acetate
  2. washThe extract was washed with saturated brine
  3. dry with materialdried over magnesium sulfate
  4. concentrationconcentrated under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-0af3bb64acb847fab8f831589a93f56d
Quelldatensatz
uspto-grants-2015_05
Patentnummer
US09023858B2

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