2-Acetylpyridine → HCID 86589146, Verbindung

HRID 2216942Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2216942
[C:1]([C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][N:5]=1)(=O)[CH3:2].[CH2:10]([N:12]1[C:16]2[CH:17]=[CH:18][CH:19]=[CH:20][C:15]=2[N:14]=[C:13]1[NH:21][NH2:22])[CH3:11]>CO.C(O)(=O)C>[CH2:10]([N:12]1[C:16]2[CH:17]=[CH:18][CH:19]=[CH:20][C:15]=2[N:14]=[C:13]1[NH:21][N:22]=[C:1]([C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][N:5]=1)[CH3:2])[CH3:11]

Komponenten

5

Edukt 2

HCID 142862-AcetylpyridineHCID 15222641-Ethyl-2-hydrazino-1H-benzimidazole

Produkt 1

HCID 86589146HCID 86589146, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 176Acetic AcidKatalysatorHCID 887MethanolLösungsmittel

Versuchsvorschrift

A mixture of 2-acetyl pyridine (0.62 g, 5.11 mmol) and 1-ethyl-2-hydrazinobenzimidazole (0.90 g, 5.11 mmol) in 20 ml of methanol is stirred at room temperature for 24 hours after the addition of 6 drops of glacial acetic acid. The reaction is monitored 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 for 24 hours in the refrigerator at approximately 5° C. The precipitate is filtered, washed several times with 50% methanol and dried. The product is recrystallized from a mixture of methanol and water. Yield: 0.99 g (70% of theory).

Aufarbeitung

  1. washThe reaction is monitored by means of thin layer chromatography (Polygram Sil G/UV254 prefabricated foils; eluting agent: CH2Cl2:MeOH (12:1))
  2. additionSubsequently, the reaction mixture is diluted with distilled water until a precipitate forms
  3. waitstored for 24 hours in the refrigerator at approximately 5° C
  4. filtrationThe precipitate is filtered
  5. washwashed several times with 50% methanol
  6. customdried
  7. customThe product is recrystallized from a mixture of methanol and water

Quellen und Nachweise

ORD-Eintrag
ord-ba46a12e3b0d4f6eb29ecd1636660287
Quelldatensatz
uspto-grants-2006_09
Patentnummer
US07112680B2

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