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Trifluoroacetic acid → HCID 11401990, Verbindung

HRID 559474
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 559474
C(OC(=O)[NH:7][C@@H:8]1[CH2:12][CH2:11][N:10]([C:13]2[CH:18]=[CH:17][C:16]([C:19]([F:22])([F:21])[F:20])=[CH:15][N:14]=2)[CH2:9]1)(C)(C)C.FC(F)(F)C(O)=O>C(Cl)Cl>[F:22][C:19]([F:20])([F:21])[C:16]1[CH:17]=[CH:18][C:13]([N:10]2[CH2:11][CH2:12][C@@H:8]([NH2:7])[CH2:9]2)=[N:14][CH:15]=1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

4

Edukt 2

HCID 6422Trifluoroacetic acidHCID 29945537(R)-N-Boc-1-(5-(trifluoromethyl)pyridin-2-yl)pyrrolidin-3-amine

Produkt 1

HCID 11401990HCID 11401990, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

A solution of D1 (11.5 g, 0.04 mol) in DCM (80 ml) was cooled (ice-bath) and trifluoroacetic acid (excess, 50 ml) was added. Reaction was warmed to ambient temperature, stirred for 3 h and partitioned between ethyl acetate and aqueous sodium hydroxide. The organic phase was separated, dried (MgSO4) and filtered. Removal of solvent under reduced pressure afforded the crude product as a yellow oil. Bulb to bulb distillation under reduced pressure initially afforded the title compound as an oil which crystallised on standing.

Aufarbeitung

  1. additionwas added
  2. customReaction
  3. custompartitioned between ethyl acetate and aqueous sodium hydroxide
  4. customThe organic phase was separated
  5. dry with materialdried (MgSO4)
  6. filtrationfiltered
  7. customRemoval of solvent under reduced pressure
  8. customafforded the crude product as a yellow oil
  9. distillationBulb to bulb distillation under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-6b558353ed4c4236bb098433e83f75dd
Quelldatensatz
uspto-grants-2011_11
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08063078B2

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