HCID 67454416, Verbindung → HCID 67456175, Verbindung

HRID 1713265Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1713265
C([O:8][C:9]1[CH:10]=[C:11]([C:15]2[CH:20]=[CH:19][C:18]([CH2:21][NH:22][C:23](=[O:29])[O:24][C:25]([CH3:28])([CH3:27])[CH3:26])=[CH:17][CH:16]=2)[CH:12]=[CH:13][CH:14]=1)C1C=CC=CC=1>C(O)C.O1CCCC1.[Pd]>[OH:8][C:9]1[CH:10]=[C:11]([C:15]2[CH:20]=[CH:19][C:18]([CH2:21][NH:22][C:23](=[O:29])[O:24][C:25]([CH3:27])([CH3:26])[CH3:28])=[CH:17][CH:16]=2)[CH:12]=[CH:13][CH:14]=1

Komponenten

4

Edukt 1

HCID 67454416HCID 67454416, Verbindung

Produkt 1

HCID 67456175HCID 67456175, VerbindungAusbeute 82 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 23938PalladiumKatalysatorHCID 21873804Tetrahydrofuran ethanolLösungsmittel

Reaktionsbedingungen

Temperatur
30 °C

Versuchsvorschrift

To a solution of tert-butyl N-(3′-bezyloxy-biphenyl-4-ylmethyl)carbamate (1.16 g) in ethanol/tetrahydrofuran (4/1, 30 mL) was added 10% palladium-on carbon (55.4 wt % H2O, 0.520 g), and the resulting mixture was stirred at 30° C. for 5 hours under a hydrogen atmosphere. The insoluble material was filtered out and the filtrate was concentrated under reduced pressure. The residue was purified by column chromatography on silica gel (eluent: hexane/ethyl acetate=5/2) to give the title compound (0.731 g).

Aufarbeitung

  1. filtrationThe insoluble material was filtered out
  2. concentrationthe filtrate was concentrated under reduced pressure
  3. customThe residue was purified by column chromatography on silica gel (eluent: hexane/ethyl acetate=5/2)

Quellen und Nachweise

ORD-Eintrag
ord-55b5c87d9b5e4a63b67cc51314548f97
Quelldatensatz
uspto-grants-2010_09
Patentnummer
US07795236B2

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