Triphenylphosphine → HCID 178508341, Verbindung

HRID 646731Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 646731
[C:1]1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.[NH2:20][C:21]1[N:22]=[CH:23][C:24]([C:38]2[CH:39]=[C:40]([CH2:44]O)[CH:41]=[CH:42][CH:43]=2)=[N:25][C:26]=1[C:27]1[NH:31][C:30]([C:32]2[CH:37]=[CH:36][CH:35]=[CH:34][CH:33]=2)=[N:29][N:28]=1.[C@@H:46]1([NH:55][S:56]([C:59]2[CH:64]=[CH:63][C:62]([N+:65]([O-:67])=[O:66])=[CH:61][C:60]=2[N+:68]([O-:70])=[O:69])(=[O:58])=[O:57])[C:54]2[C:49](=[CH:50][CH:51]=[CH:52][CH:53]=2)[CH2:48][CH2:47]1.N(C(OCC)=O)=NC(OCC)=O>C1COCC1.C(OCC)(=O)C>[NH2:20][C:21]1[N:22]=[CH:23][C:24]([C:38]2[CH:39]=[C:40]([CH:41]=[CH:42][CH:43]=2)[CH2:44][N:55]([C@@H:46]2[C:54]3[C:49](=[CH:50][CH:51]=[CH:52][CH:53]=3)[CH2:48][CH2:47]2)[S:56]([C:59]2[CH:64]=[CH:63][C:62]([N+:65]([O-:67])=[O:66])=[CH:61][C:60]=2[N+:68]([O-:70])=[O:69])(=[O:58])=[O:57])=[N:25][C:26]=1[C:27]1[NH:31][C:30]([CH2:32][C:33]2[CH:1]=[CH:37][CH:36]=[CH:35][CH:34]=2)=[N:29][N:28]=1

Komponenten

7

Edukt 4

HCID 11776TriphenylphosphineHCID 220568ethyl N-ethoxycarbonyliminocarbamateHCID 86607845N-[(1S)-2,3-dihydro-1H-inden-1-yl]-2,4-dinitrobenzen sulfonamideHCID 178508343HCID 178508343, Verbindung

Produkt 1

HCID 178508341HCID 178508341, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 8028TetrahydrofuranLösungsmittelHCID 8857Ethyl AcetateLösungsmittel

Versuchsvorschrift

Triphenylphosphine (47 mg, 0.17 mmol) was added to a stirred solution of {3-[5-amino-6-(5-phenyl-4H-1,2,4-triazol-3-yl) pyrazine-2-yl]phenyl}methanol (50 mg, 0.14 mmol) and N-[(1S)-2,3-dihydro-1H-inden-1-yl]-2,4-dinitrobenzen sulfonamide (60 mg, 0.16 mmol) in THF. Diethyl azodicarboxylate (31 mg, 0.17 mmol) was then added and mixture was stirred at ambient temperature 4 h. Ethyl acetate (20 mL) was added, and the organic layer was washed with saturated aqueous sodium chloride, and then dried (Na2SO4). Filtration and concentration followed by chromatography on silica gel afforded the title compound: MS (EI) for C35H29N9O6S: 704 (MH+).

Aufarbeitung

  1. washthe organic layer was washed with saturated aqueous sodium chloride
  2. dry with materialdried (Na2SO4)
  3. filtrationFiltration and concentration

Quellen und Nachweise

ORD-Eintrag
ord-0dfe80fcffe04a9cacdd4cee45d0e875
Quelldatensatz
uspto-grants-2010_04
Patentnummer
US07704995B2

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