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Potassium Acetate → HCID 58355527, Verbindung

HRID 2169027
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 2169027
Cl[C:2]1[N:3]=[C:4]([C:41]2[CH:46]=[CH:45][CH:44]=[CH:43][CH:42]=2)[N:5]([CH2:35][CH2:36][CH2:37][CH2:38][O:39][CH3:40])[C:6]=1[C:7]([N:9]([CH2:31][CH:32]([CH3:34])[CH3:33])[C@H:10]1[CH2:15][C@@H:14]([C:16]([N:18]2[CH2:23][CH2:22][O:21][CH2:20][CH2:19]2)=[O:17])[CH2:13][N:12]([C:24]([O:26][C:27]([CH3:30])([CH3:29])[CH3:28])=[O:25])[CH2:11]1)=[O:8].C([O-])(=O)C.[K+]>CO.[OH-].[Pd+2].[OH-].[C]>[CH3:40][O:39][CH2:38][CH2:37][CH2:36][CH2:35][N:5]1[C:6]([C:7]([N:9]([CH2:31][CH:32]([CH3:33])[CH3:34])[C@H:10]2[CH2:15][C@@H:14]([C:16]([N:18]3[CH2:19][CH2:20][O:21][CH2:22][CH2:23]3)=[O:17])[CH2:13][N:12]([C:24]([O:26][C:27]([CH3:30])([CH3:28])[CH3:29])=[O:25])[CH2:11]2)=[O:8])=[CH:2][N:3]=[C:4]1[C:41]1[CH:42]=[CH:43][CH:44]=[CH:45][CH:46]=1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 2

HCID 517044Potassium AcetateHCID 58355151HCID 58355151, Verbindung

Produkt 1

HCID 58355527HCID 58355527, VerbindungAusbeute 47,5 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 178502593HCID 178502593, VerbindungKatalysatorHCID 887MethanolLösungsmittel

Versuchsvorschrift

tert-Butyl (3S,5R)-3-[{[4-chloro-1-(4-methoxybutyl)-2-phenyl-1H-imidazol-5-yl]carbonyl}(2-methylpropyl)amino]-5-(morpholin-4-ylcarbonyl)piperidine-1-carboxylate (200 mg), palladium(II) hydroxide-carbon (20 mg) and potassium acetate (30 mg) were suspended in methanol (10 ml), and the mixture was stirred under a hydrogen atmosphere (1 atom) at room temperature for 1 day. The palladium catalyst was filtered off and the filtrate was concentrated under reduced pressure. The residue was suspended in water, and the suspension was extracted with ethyl acetate. The extract was washed with saturated brine, and dried over anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure. The residue was subjected to silica gel column chromatography, and a fraction eluted with ethyl acetate-hexane (10:90-80:20) was concentrated under reduced pressure to give the object product (90 mg).

Aufarbeitung

  1. filtrationThe palladium catalyst was filtered off
  2. concentrationthe filtrate was concentrated under reduced pressure
  3. extractionthe suspension was extracted with ethyl acetate
  4. washThe extract was washed with saturated brine
  5. dry with materialdried over anhydrous magnesium sulfate
  6. customThe solvent was evaporated under reduced pressure
  7. washa fraction eluted with ethyl acetate-hexane (10:90-80:20)
  8. concentrationwas concentrated under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-fff0af94bc704610a4e1fa2de1393a77
Quelldatensatz
uspto-grants-2015_06
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US09045436B2

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