Water → HCID 66816082, Verbindung

HRID 1754917Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1754917
C([O-])([O-])=O.[K+].[K+].[C:7]([N:10]([C:17]1[CH:22]=[CH:21][C:20]([CH2:23][CH2:24][S:25]([N:28]2[CH2:49][CH2:48][C:31]3([N:35]=[C:34]([C:36]4[CH:41]=[CH:40][CH:39]=[C:38]([O:42][C:43]([F:46])([F:45])[F:44])[CH:37]=4)[NH:33][C:32]3=[O:47])[CH2:30][CH2:29]2)(=[O:27])=[O:26])=[C:19]([CH3:50])[CH:18]=1)[CH2:11][CH2:12][O:13]C(=O)C)(=[O:9])[CH3:8].O>CO.C(Cl)Cl>[OH:13][CH2:12][CH2:11][N:10]([C:17]1[CH:22]=[CH:21][C:20]([CH2:23][CH2:24][S:25]([N:28]2[CH2:49][CH2:48][C:31]3([N:35]=[C:34]([C:36]4[CH:41]=[CH:40][CH:39]=[C:38]([O:42][C:43]([F:45])([F:46])[F:44])[CH:37]=4)[NH:33][C:32]3=[O:47])[CH2:30][CH2:29]2)(=[O:27])=[O:26])=[C:19]([CH3:50])[CH:18]=1)[C:7](=[O:9])[CH3:8]

Komponenten

6

Edukt 3

HCID 962WaterHCID 11430Potassium CarbonateHCID 66816902Acetic acid 2-[acetyl-(3-methyl-4-{2-[4-oxo-2-(3-trifluoromethoxy-phenyl)-1,3,8-triaza-spiro[4.5]dec-1-ene-8-sulfonyl]-ethyl}-phenyl)-amino]-ethyl ester

Produkt 1

HCID 66816082HCID 66816082, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 887MethanolLösungsmittelHCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

K2CO3 (9.1 mg, 66.0 μmol) was added to a solution of acetic acid 2-[acetyl-(3-methyl-4-{2-[4-oxo-2-(3-trifluoromethoxy-phenyl)-1,3,8-triaza-spiro[4.5]dec-1-ene-8-sulfonyl]-ethyl}-phenyl)-amino]-ethyl ester (28.1 mg, 44.0 μmol) in MeOH (0.5 mL). The mixture was stirred at room temperature for two hours. H2O was then added and the mixture was diluted with CH2Cl2. The organic layer was washed with saturated brine, and then dried over MgSO4 and concentrated under reduced pressure. The resulting residue was purified by column chromatography (CH2Cl2/MeOH=15/1) to give N-(2-hydroxy-ethyl)-N-(3-methyl-4-{2-[4-oxo-2-(3-trifluoromethoxy-phenyl)-1,3,8-triaza-spiro[4.5]dec-1-ene-8-sulfonyl]-ethyl}-phenyl)-acetamide as a white amorphous (24.0 mg, 92%).

Aufarbeitung

  1. washThe organic layer was washed with saturated brine
  2. dry with materialdried over MgSO4
  3. concentrationconcentrated under reduced pressure
  4. customThe resulting residue was purified by column chromatography (CH2Cl2/MeOH=15/1)

Quellen und Nachweise

ORD-Eintrag
ord-c6173fa8dc6b4d54902ebe6cbecdd332
Quelldatensatz
uspto-grants-2015_10
Patentnummer
US09169254B2

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