Sodium Hydroxide → N-(3-{6-[1-(4-Methoxybenzyl)-1H-pyrazol-4-yl]-1H-imidazo[1,2-b]pyrazol-1-yl}-4-methyl-phenyl)-3-(4-methylpiperazin-1-yl)-5-(pentafluoro-lambda6-sulphanyl)benzamide

HRID 1055665Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1055665
F[C:2](F)(F)[C:3]([OH:5])=O.COC1C=CC([CH2:14][N:15]2[CH:19]=[C:18]([C:20]3[CH:21]=[C:22]4[N:27]([C:28]5[CH:29]=[C:30]([CH:32]=[CH:33][C:34]=5[CH3:35])[NH2:31])[CH:26]=[CH:25][N:23]4[N:24]=3)[CH:17]=[N:16]2)=CC=1.F[C:39](F)(F)C(O)=O.[CH3:45][N:46]1[CH2:51][CH2:50][N:49]([C:52]2[CH:53]=[C:54]([CH:58]=[C:59]([S:61]([F:66])([F:65])([F:64])([F:63])[F:62])[CH:60]=2)[C:55]([OH:57])=O)[CH2:48][CH2:47]1.CN(C(ON1N=N[C:77]2[CH:78]=[CH:79]C=N[C:76]1=2)=[N+](C)C)C.F[P-](F)(F)(F)(F)F.C(N(CC)C(C)C)(C)C.[OH-].[Na+]>CN(C=O)C>[CH3:39][O:5][C:3]1[CH:2]=[CH:79][C:78]([CH2:14][N:15]2[CH:19]=[C:18]([C:20]3[CH:21]=[C:22]4[N:27]([C:28]5[CH:29]=[C:30]([NH:31][C:55](=[O:57])[C:54]6[CH:58]=[C:59]([S:61]([F:62])([F:63])([F:65])([F:64])[F:66])[CH:60]=[C:52]([N:49]7[CH2:48][CH2:47][N:46]([CH3:45])[CH2:51][CH2:50]7)[CH:53]=6)[CH:32]=[CH:33][C:34]=5[CH3:35])[CH:26]=[CH:25][N:23]4[N:24]=3)[CH:17]=[N:16]2)=[CH:77][CH:76]=1

Komponenten

7

Edukt 5

HCID 14798Sodium HydroxideHCID 81531DiisopropylethylamineHCID 9886157Methanaminium, N-((dimethylamino)(3H-1,2,3-triazolo(4,5-b)pyridin-3-yloxy)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1)HCID 896995603-(4-Methylpiperazin-1-yl)-5-(pentafluoro-lambda6-sulphanyl)benzoic acid trifluoroacetateHCID 897000263-{6-[1-(4-Methoxybenzyl)-1H-pyrazol-4-yl]-1H-imidazo[1,2-b]pyrazol-1-yl}-4-methylaniline trifluoroacetate

Produkt 1

HCID 89699916N-(3-{6-[1-(4-Methoxybenzyl)-1H-pyrazol-4-yl]-1H-imidazo[1,2-b]pyrazol-1-yl}-4-methyl-phenyl)-3-(4-methylpiperazin-1-yl)-5-(pentafluoro-lambda6-sulphanyl)benzamide

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel

Versuchsvorschrift

70 mg (0.14 mmol) of the compound of Example 8A, 62.9 mg (0.14 mmol) of the compound of Example 17A and 62 mg (0.16 mmol) of HATU were dissolved in 0.79 ml of DMF, 0.07 ml (0.41 mmol) of N,N-diisopropylethylamine were added and the mixture was stirred at RT for 1 h. The mixture was then stirred into 10 ml of 0.1 M aqueous sodium hydroxide solution and stirred at RT for 10 min, and the precipitate formed was then filtered off. The solid was washed with water and dried under high vacuum. This gave 94 mg (94% pure, 89% of theory) of the title compound.

Aufarbeitung

  1. stirringstirred at RT for 10 min
  2. customthe precipitate formed
  3. filtrationwas then filtered off
  4. washThe solid was washed with water
  5. customdried under high vacuum

Quellen und Nachweise

ORD-Eintrag
ord-80d46318b41c4c0c897b2fec4d9376a0
Quelldatensatz
uspto-grants-2016_07
Patentnummer
US09394309B2

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