Ammonium formate → HCID 70001232, Verbindung

HRID 1634795Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1634795
C([O:3][C:4](=[O:41])[C:5]1[CH:10]=[CH:9][C:8]([NH:11][C:12]([N:14]2[CH2:19][CH2:18][CH:17]([CH2:20][NH:21][CH2:22][C@H:23]([OH:40])[CH2:24][O:25][C:26]3[CH:31]=[CH:30][C:29]([O:32][CH2:33][C:34]4[CH:39]=[CH:38][CH:37]=[CH:36][CH:35]=4)=[CH:28][CH:27]=3)[CH2:16][CH2:15]2)=[O:13])=[CH:7][CH:6]=1)C.C([O-])=O.[NH4+]>CO.[Pd]>[OH:40][C@H:23]([CH2:24][O:25][C:26]1[CH:31]=[CH:30][C:29]([O:32][CH2:33][C:34]2[CH:35]=[CH:36][CH:37]=[CH:38][CH:39]=2)=[CH:28][CH:27]=1)[CH2:22][NH:21][CH2:20][CH:17]1[CH2:16][CH2:15][N:14]([C:12]([NH:11][C:8]2[CH:9]=[CH:10][C:5]([C:4]([OH:41])=[O:3])=[CH:6][CH:7]=2)=[O:13])[CH2:19][CH2:18]1

Komponenten

5

Edukt 2

HCID 2723923Ammonium formateHCID 69999017HCID 69999017, Verbindung

Produkt 1

HCID 70001232HCID 70001232, VerbindungAusbeute 26,6 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 23938PalladiumKatalysatorHCID 887MethanolLösungsmittel

Versuchsvorschrift

A mixture of 4-[(4-{[(2S)-2-hydroxy-3-(4-benzyloxy-phenoxy)-propylamino]-methyl}-piperidine-1-carbonyl)-amino]-benzoic acid ethyl ester (0.11 g, 0.43 mmol) and ammonium formate (0.063 g, 1 mmol) in 5 mL of methanol over 0.110 g of 10% palladium on carbon was stirred at ambient temperature overnight. The catalyst was filtered (solka floc) and the filtrate concentrated in vacuo. Trituration of the crude solid foam with Et2O provided 0.061 g of the title compound as a white solid.

Aufarbeitung

  1. filtrationThe catalyst was filtered (solka floc)
  2. concentrationthe filtrate concentrated in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-d3a51b463ce64ed181a51d0847bfb172
Quelldatensatz
uspto-grants-2003_01
Patentnummer
US06506901B2

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