Trifluoroacetic acid → 1-(4-Diisopropylaminomethylbenzoyl)piperazine

HRID 278549Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 278549
C(OC([N:8]1[CH2:13][CH2:12][N:11]([C:14](=[O:29])[C:15]2[CH:20]=[CH:19][C:18]([CH2:21][N:22]([CH:26]([CH3:28])[CH3:27])[CH:23]([CH3:25])[CH3:24])=[CH:17][CH:16]=2)[CH2:10][CH2:9]1)=O)(C)(C)C.FC(F)(F)C(O)=O>C(OCC)(=O)C>[CH:23]([N:22]([CH2:21][C:18]1[CH:19]=[CH:20][C:15]([C:14]([N:11]2[CH2:12][CH2:13][NH:8][CH2:9][CH2:10]2)=[O:29])=[CH:16][CH:17]=1)[CH:26]([CH3:28])[CH3:27])([CH3:24])[CH3:25]

Komponenten

4

Edukt 2

HCID 6422Trifluoroacetic acidHCID 226280611-(Tert-butoxycarbonyl)-4-(4-diisopropylaminomethylbenzoyl)piperazine

Produkt 1

HCID 226279521-(4-Diisopropylaminomethylbenzoyl)piperazineAusbeute 90,2 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8857Ethyl AcetateLösungsmittel

Versuchsvorschrift

To a solution of 1-(tert-butoxycarbonyl)-4-(4-diisopropylaminomethylbenzoyl)piperazine (4.6 g) in ethyl acetate (10 ml) was added trifluoroacetic acid (20 ml), and the solution was stirred at room temperature for 1 hour and concentrated. The residue was dissolved in water. The solution was made alkaline with sodium hydroxide solution, extracted with dichloromethane. The extract was dried and concentrated to give amorphous powders which were filtered, washed with hexane and dried to afford the title compound (3.12 g).

Aufarbeitung

  1. concentrationconcentrated
  2. dissolutionThe residue was dissolved in water
  3. extractionextracted with dichloromethane
  4. customThe extract was dried
  5. concentrationconcentrated
  6. customto give amorphous powders which
  7. filtrationwere filtered
  8. washwashed with hexane
  9. customdried

Quellen und Nachweise

ORD-Eintrag
ord-084ef76c38a54aa4b696a7f2a3824efa
Quelldatensatz
uspto-grants-2002_03
Patentnummer
US06359134B1

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