Ethanol → 3-[5-(2-Amino-pyrimidin-5-yl)-1-tert-butyl-1H-benzimidazol-2-yl]-4-1,2,4-triazol-1-yl-benzoic acid
Reaktionsgleichung
[NH2:1][C:2]1[N:7]=[CH:6][C:5]([C:8]2[CH:33]=[CH:32][C:11]3[N:12]([C:28]([CH3:31])([CH3:30])[CH3:29])[C:13]([C:15]4[CH:16]=C([CH:20]=[CH:21][C:22]=4[N:23]4[CH:27]=[N:26][CH:25]=[N:24]4)C#N)=[N:14][C:10]=3[CH:9]=2)=[CH:4][N:3]=1.[OH-:34].[K+].[CH3:36][CH2:37][OH:38]>O>[NH2:1][C:2]1[N:7]=[CH:6][C:5]([C:8]2[CH:33]=[CH:32][C:11]3[N:12]([C:28]([CH3:31])([CH3:30])[CH3:29])[C:13]([C:15]4[CH:16]=[C:36]([CH:20]=[CH:21][C:22]=4[N:23]4[CH:27]=[N:26][CH:25]=[N:24]4)[C:37]([OH:34])=[O:38])=[N:14][C:10]=3[CH:9]=2)=[CH:4][N:3]=1Komponenten
5
Edukt 3
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 1
Reaktionsbedingungen
- Temperatur
- 80 °C
Versuchsvorschrift
To a mixture of 3-[5-(2-amino-pyrimidin-5-yl)-1-tert-butyl-1H-benzimidazol-2-yl]-4-1,2,4-triazol-1-yl-benzonitrile (Example 7) (400 mg, 0.92 mmol) in EtOH (10 mL) is added KOH (103 mg, 1.8 mmol) in H2O (1 mL) at room temperature. The mixture is heated to 80° C. for 48 hours. The solution is cooled down and is concentrated under vacuum. The residue is dissolved in H2O (10 mL) and the pH of the solution is adjusted to 6 with 2M HCl solution. The white solid that precipitates out from the solution is collected by filtration. The white solid is dried under vacuum providing the title compound. LCMS (ESMS): m/z 455.20 (M++1)
Aufarbeitung
- temperatureThe solution is cooled down
- concentrationis concentrated under vacuum
- dissolutionThe residue is dissolved in H2O (10 mL)
- customThe white solid that precipitates out from the solution
- filtrationis collected by filtration
- customThe white solid is dried under vacuum
Quellen und Nachweise
- ORD-Eintrag
- ord-354e54afbd2d4a1c9f4d849a813b6673
- Quelldatensatz
- uspto-grants-2013_04
- Patentnummer
- US08420655B2
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