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Succinic anhydride → HCID 59324177, Verbindung

HRID 508121
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 508121
[F:1][C:2]([F:8])([F:7])[C:3]1([NH2:6])[CH2:5][CH2:4]1.C(N(C(C)C)CC)(C)C.[C:18]1(=[O:24])[O:23][C:21](=[O:22])[CH2:20][CH2:19]1>O1CCOCC1>[O:24]=[C:18]([NH:6][C:3]1([C:2]([F:8])([F:7])[F:1])[CH2:5][CH2:4]1)[CH2:19][CH2:20][C:21]([OH:23])=[O:22]
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 3

HCID 7922Succinic anhydrideHCID 81531DiisopropylethylamineHCID 116511971-(Trifluoromethyl)cyclopropanamine

Produkt 1

HCID 59324177HCID 59324177, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 312751,4-DioxaneLösungsmittel

Reaktionsbedingungen

Temperatur
10 °C

Versuchsvorschrift

Slowly, 800.7 mg (4.96 mmol) of 1-(trifluoromethyl)cyclopropanamine and 0.85 ml (4.96 mmol) of diisopropylethylamine were added to a solution of 496 mg (4.96 mmol) of succinic anhydride in 10 ml of dioxane, with ice-cooling (10° C.). Stirring was continued for 20 min at room temperature, and the mixture was allowed to stand overnight at this temperature. Again, stirring was continued for 20 min at 80° C., the mixture was allowed to cool to room temperature, and the solution was concentrated. Repeatedly, the solution was washed alternately with ethyl acetate and with water. The combined organic phases were dried and concentrated. This gave 815.8 mg (73% of theory) of the desired compound.

Aufarbeitung

  1. waitto stand overnight at this temperature
  2. stirringAgain, stirring
  3. waitwas continued for 20 min at 80° C.
  4. temperatureto cool to room temperature
  5. concentrationthe solution was concentrated
  6. washRepeatedly, the solution was washed alternately with ethyl acetate and with water
  7. customThe combined organic phases were dried
  8. concentrationconcentrated

Quellen und Nachweise

ORD-Eintrag
ord-a35ca9a1533c4bfa8b56a7f8e3bdef7b
Quelldatensatz
uspto-grants-2015_08
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US09095140B2

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