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Sodium Carbonate → HCID 73426448, Verbindung

HRID 1507558
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1507558
[CH3:1][N:2]1[CH:6]=[CH:5][N:4]=[C:3]1[C:7]([OH:9])=O.[NH2:10][C:11]1[CH:19]=[C:18]2[C:14]([C:15]([CH3:23])([CH3:22])[C:16](=[O:21])[N:17]2[CH3:20])=[CH:13][CH:12]=1.CN(C(ON1N=NC2C=CC=NC1=2)=[N+](C)C)C.F[P-](F)(F)(F)(F)F.CCN(C(C)C)C(C)C.C(=O)([O-])[O-].[Na+].[Na+]>CN(C=O)C.C(OCC)(=O)C>[CH3:1][N:2]1[CH:6]=[CH:5][N:4]=[C:3]1[C:7]([NH:10][C:11]1[CH:19]=[C:18]2[C:14]([C:15]([CH3:23])([CH3:22])[C:16](=[O:21])[N:17]2[CH3:20])=[CH:13][CH:12]=1)=[O:9]
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Komponenten

8

Edukt 5

HCID 10340Sodium CarbonateHCID 81531DiisopropylethylamineHCID 5576781-methyl-1H-imidazole-2-carboxylic acidHCID 9886157Methanaminium, N-((dimethylamino)(3H-1,2,3-triazolo(4,5-b)pyridin-3-yloxy)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1)HCID 529112486-Amino-1,3,3-trimethyl-1,3-dihydro-2H-indol-2-one

Produkt 1

HCID 73426448
HCID 73426448, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 6228DimethylformamideLösungsmittelHCID 8857Ethyl AcetateLösungsmittel

Versuchsvorschrift

To a solution of 1-methyl-1H-imidazole-2-carboxylic acid (99.4 mg, 788 μmol) and 6-amino-1,3,3-trimethylindolin-2-one (100 mg, 526 μmol) in DMF (3 ml) were added HATU (400 mg, 1.05 mmol) and DIPEA (347 mg, 468 μl, 2.63 mmol). The reaction mixture was stirred for 3 hours at room temperature and then poured into ethyl acetate and 1 M aqueous sodium carbonate solution. The aqueous phase was extracted with ethyl acetate. The combined organic layers were dried over sodium sulfate and the solvent was removed under reduced pressure. The crude material was purified by silica gel chromatography using ethyl acetate/heptane as eluent followed by reversed phase preparative HPLC. The title compound was obtained as off-white crystals (135 mg).

Aufarbeitung

  1. extractionThe aqueous phase was extracted with ethyl acetate
  2. dry with materialThe combined organic layers were dried over sodium sulfate
  3. customthe solvent was removed under reduced pressure
  4. customThe crude material was purified by silica gel chromatography

Quellen und Nachweise

ORD-Eintrag
ord-ae0a3ff2b1c24a64a750c29710c90868
Quelldatensatz
uspto-grants-2015_12
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US09221816B2

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