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Trifluoroacetic acid → HCID 58118717, Verbindung

HRID 1866668
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1866668
[F:1][C:2]1[CH:3]=[C:4]([C@H:9]2[N:14](C(OC(C)(C)C)=O)[C:13](=[O:22])[C:12]([CH2:25][CH3:26])([CH2:23][CH3:24])[CH2:11][CH2:10]2)[CH:5]=[C:6]([F:8])[CH:7]=1.C(O)(C(F)(F)F)=O>C(Cl)Cl>[F:1][C:2]1[CH:3]=[C:4]([C@H:9]2[NH:14][C:13](=[O:22])[C:12]([CH2:25][CH3:26])([CH2:23][CH3:24])[CH2:11][CH2:10]2)[CH:5]=[C:6]([F:8])[CH:7]=1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

4

Edukt 2

HCID 6422Trifluoroacetic acidHCID 66864622HCID 66864622, Verbindung

Produkt 1

HCID 58118717HCID 58118717, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

To a solution of tert-butyl (6S)-6-(3,5-difluorophenyl)-3,3-diethylpiperidin-2-one-1-carboxylate from Step D (1.22 g, 3.32 mmol) in CH2Cl2 (7 mL) at ambient temperature was added TFA (3 mL). After stirring for 1.5 h, the reaction mixture was concentrated in vacuo. The residue was partitioned between CH2Cl2 (30 mL) and saturated NaHCO3 (30 mL). The layers were separated and the aqueous layer was further extracted with CH2Cl2 (2×30 mL). The combined organics were dried over sodium sulfate, filtered and then concentrated in vacuo to provide the title compound, which could be used without further purification. MS: m/z=268 (M+1).

Aufarbeitung

  1. concentrationthe reaction mixture was concentrated in vacuo
  2. customThe residue was partitioned between CH2Cl2 (30 mL) and saturated NaHCO3 (30 mL)
  3. customThe layers were separated
  4. extractionthe aqueous layer was further extracted with CH2Cl2 (2×30 mL)
  5. dry with materialThe combined organics were dried over sodium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-71a6ea55c3a446d382539158fc8246a2
Quelldatensatz
uspto-grants-2009_12
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US07629338B2

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