Triethylamine → 2-(3-Oxo-6-pyridin-4-yl-2,3-dihydropyridazin-4-yl)-1H-benzimidazole-5-carboxylic acid (2-diethylaminoethyl)amide

HRID 2354576

Reaktionsgleichung

Reaktionsgleichung von HRID 2354576
[O:1]=[C:2]1[C:7]([C:8]2[NH:9][C:10]3[CH:16]=[C:15]([C:17]([OH:19])=O)[CH:14]=[CH:13][C:11]=3[N:12]=2)=[CH:6][C:5]([C:20]2[CH:25]=[CH:24][N:23]=[CH:22][CH:21]=2)=[N:4][NH:3]1.C(N(CC)CC)C.F[P-](F)(F)(F)(F)F.N1(OC(N(C)C)=[N+](C)C)C2N=CC=CC=2N=N1.[CH2:57]([N:59]([CH2:62][CH2:63][NH2:64])[CH2:60][CH3:61])[CH3:58]>O.CN(C)C=O>[CH2:57]([N:59]([CH2:60][CH3:61])[CH2:62][CH2:63][NH:64][C:17]([C:15]1[CH:14]=[CH:13][C:11]2[NH:12][C:8]([C:7]3[C:2](=[O:1])[NH:3][N:4]=[C:5]([C:20]4[CH:21]=[CH:22][N:23]=[CH:24][CH:25]=4)[CH:6]=3)=[N:9][C:10]=2[CH:16]=1)=[O:19])[CH3:58]

Komponenten

7

Edukt 4

HCID 8471TriethylamineHCID 60993N,N-DiethylethylenediamineHCID 9886157Methanaminium, N-((dimethylamino)(3H-1,2,3-triazolo(4,5-b)pyridin-3-yloxy)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1)HCID 1360781992-(3-oxo-6-pyridin-4-yl-2,3-dihydropyridazin-4-yl)-1H-benzoimidazole-5-carboxylic acid

Produkt 1

HCID 1784640622-(3-Oxo-6-pyridin-4-yl-2,3-dihydropyridazin-4-yl)-1H-benzimidazole-5-carboxylic acid (2-diethylaminoethyl)amide

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 962WaterLösungsmittelHCID 6228DimethylformamideLösungsmittel

Versuchsvorschrift

A mixture consisting of 50 mg of 2-(3-oxo-6-pyridin-4-yl-2,3-dihydropyridazin-4-yl)-3H-benzoimidazole-5-carboxylic acid, 0.065 ml of triethylamine and 1.5 ml of dimethylformamide (DMF) is stirred at room temperature for 10 minutes, mixed with 68.4 mg of O-(7-azabenzotriazol-1-yl)-N,N,N′,N′-tetramethyluronium hexafluorophosphate (Hatu) and stirred at room temperature for a further 30 minutes. Then 21 mg of diethylaminoethylamine are added, and the mixture is stirred at 50° C. for 3 hours. After cooling, it is diluted with 5 ml of water, and the precipitate is filtered off with suction and stirred with isopropanol at 60° C., filtered off with suction and dried in vacuo.

Aufarbeitung

  1. stirringstirred at room temperature for a further 30 minutes
  2. stirringthe mixture is stirred at 50° C. for 3 hours
  3. temperatureAfter cooling
  4. filtrationthe precipitate is filtered off with suction
  5. stirringstirred with isopropanol at 60° C.
  6. filtrationfiltered off with suction
  7. customdried in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-a82d10d4d0f54373a04355142e2f5524
Quelldatensatz
uspto-grants-2010_07
Patentnummer
US07754713B2

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