Lithium Hydroxide → HCID 11671386, Verbindung

HRID 1867625Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1867625
[OH-].[Li+].[O:3]=[C:4]1[NH:8][C:7]([C:9]([O:11]C)=[O:10])=[CH:6][N:5]1[CH:13]1[CH2:18][CH2:17][N:16]([C:19]([NH:21][C@@H:22]2[N:28]=[C:27]([C:29]3[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=3)[C:26]3[CH:35]=[CH:36][CH:37]=[CH:38][C:25]=3[N:24]([CH2:39][C:40]([F:43])([F:42])[F:41])[C:23]2=[O:44])=[O:20])[CH2:15][CH2:14]1>O.CO>[O:3]=[C:4]1[NH:8][C:7]([C:9]([OH:11])=[O:10])=[CH:6][N:5]1[CH:13]1[CH2:18][CH2:17][N:16]([C:19]([NH:21][C@@H:22]2[N:28]=[C:27]([C:29]3[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=3)[C:26]3[CH:35]=[CH:36][CH:37]=[CH:38][C:25]=3[N:24]([CH2:39][C:40]([F:43])([F:42])[F:41])[C:23]2=[O:44])=[O:20])[CH2:15][CH2:14]1

Komponenten

5

Edukt 2

HCID 3939Lithium HydroxideHCID 11519899HCID 11519899, Verbindung

Produkt 1

HCID 11671386HCID 11671386, VerbindungAusbeute 17,2 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 887MethanolLösungsmittelHCID 962WaterLösungsmittel

Versuchsvorschrift

Lithium hydroxide (43 mg, 1.03 mmol) in water (2 mL) was added to a solution methyl 2-oxo-1-[1-({[(3R)-2-oxo-5-phenyl-1-(2,2,2-trifluoroethyl)-2,3-dihydro-1H-1,4-benzodiazepin-3-yl]amino}carbonyl)piperidin-4-yl]-2,3-dihydro-1H-imidazole-4-carboxylate (30 mg, 0.051 mmol) in methanol (2 mL) and heated to 40 o C. After 2 h, the reaction was purified by preparative reverse phase chromatography to give the title compound (5 mg). MS 571.2 (M+1)

Aufarbeitung

  1. temperatureheated to 40 o C
  2. customthe reaction was purified by preparative reverse phase chromatography

Quellen und Nachweise

ORD-Eintrag
ord-91151eaa579e4544a6666d159101a2d5
Quelldatensatz
uspto-grants-2009_12
Patentnummer
US07632832B2

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