HCID 67313552, Verbindung → HCID 131729000, Verbindung

HRID 1010882Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1010882
C(O[C:9](=O)[N:10]([CH2:12][C:13]([C:15]1[CH:20]=[CH:19][C:18]([C@@H:21]([NH:23][C:24]([O:26][C:27]([CH3:30])([CH3:29])[CH3:28])=[O:25])[CH3:22])=[CH:17][CH:16]=1)=[O:14])C)C1C=CC=CC=1>O1CCCC1.CO.[C].[Pd]>[C:27]([O:26][C:24](=[O:25])[NH:23][C@H:21]([C:18]1[CH:17]=[CH:16][C:15]([C:13](=[O:14])[CH2:12][NH:10][CH3:9])=[CH:20][CH:19]=1)[CH3:22])([CH3:29])([CH3:28])[CH3:30]

Komponenten

5

Edukt 1

HCID 67313552HCID 67313552, Verbindung

Produkt 1

HCID 131729000HCID 131729000, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 178418390HCID 178418390, VerbindungKatalysator2×HCID 887MethanolLösungsmittelHCID 8028TetrahydrofuranLösungsmittel

Versuchsvorschrift

159 mg of the compound [2-2] was dissolved in a mixed solvent of 4 mL of tetrahydrofuran and 2 mL of methanol, then 48 mg of 10% palladium carbon catalyst was added thereto, and the mixture was further stirred for 2 hours under hydrogen atmosphere. Thereto, 95 mg of 10% palladium carbon catalyst was further added and stirred for 3.5 hours under hydrogen atmosphere. The insolubles were filtered through celite and the filtrate was concentrated under reduced pressure, to obtain tert-butyl{(1S)-1-[4-(N-methylglycyl)phenyl]ethyl}carbamate [2-3] (hereinafter, referred to as the compound [2-3]) as crude and purified products. The compound [2-3] was used in the subsequent reaction without further purification.

Aufarbeitung

  1. stirringstirred for 3.5 hours under hydrogen atmosphere
  2. filtrationThe insolubles were filtered through celite
  3. concentrationthe filtrate was concentrated under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-ace09b96cbd6480cb26001bb573d6e38
Quelldatensatz
uspto-grants-2011_07
Patentnummer
US07977336B2

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