Reaktionsgleichung
[CH:1]1([C:4]([C:6]2[CH:11]=[CH:10][CH:9]=[CH:8][N:7]=2)=O)[CH2:3][CH2:2]1.[CH3:12][N:13]1[C:17]2[CH:18]=[CH:19][CH:20]=[CH:21][C:16]=2[N:15]=[C:14]1[NH:22][NH2:23]>CO.C(O)(=O)C>[CH3:12][N:13]1[C:17]2[CH:18]=[CH:19][CH:20]=[CH:21][C:16]=2[N:15]=[C:14]1[NH:22]/[N:23]=[C:4](/[CH:1]1[CH2:3][CH2:2]1)\[C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][N:7]=1Komponenten
5
Edukt 2
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 2
Versuchsvorschrift
A mixture of cyclopropyl-(2-pyridyl)-methanone (1,00 g, 7,40 mmol) and 1-methyl-2-hydrazinobenzimidazole (1.20 g, 7.40 mmol) in 20 ml of methanol is stirred for 3 days at room temperature after the addition of 6 drops of glacial acetic acid. Monitoring is effected by means of thin layer chromatography (Polygram Sil G/UV254 prefabricated foils; eluting agent: CH2Cl2:MeOH (12:1)). Subsequently, the reaction mixture is diluted with distilled water until a precipitate forms and stored in the refrigerator at approximately 5° C. for 24 hours. The precipitate is filtered, washed several times with 50% methanol, and dried. The product is recrystallized from a mixture of methanol and water. Yield: 0.97 g (45% of theory).
Aufarbeitung
- washMonitoring is effected by means of thin layer chromatography (Polygram Sil G/UV254 prefabricated foils; eluting agent: CH2Cl2:MeOH (12:1))
- additionSubsequently, the reaction mixture is diluted with distilled water until a precipitate forms
- waitstored in the refrigerator at approximately 5° C. for 24 hours
- filtrationThe precipitate is filtered
- washwashed several times with 50% methanol
- customdried
- customThe product is recrystallized from a mixture of methanol and water
Quellen und Nachweise
- ORD-Eintrag
- ord-33d97b1198784fbe8bfd770cbe9bb30a
- Quelldatensatz
- uspto-grants-2006_09
- Patentnummer
- US07112680B2
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