Acetic Acid → HCID 178527899, Verbindung

HRID 631944

Reaktionsgleichung

Reaktionsgleichung von HRID 631944
[Br:1][C:2]1C=C[C:5]2OCO[C:4]=2[C:3]=1C=O.[CH3:13][CH:14]([OH:16])[CH3:15].[NH2:17][C:18]1[CH:27]=[CH:26][C:21]2[NH:22][C:23](=[S:25])[NH:24][C:20]=2[CH:19]=1.[C:28](O)(=[O:30])C>>[Br:1][C:2]1[CH:3]=[C:4](/[CH:5]=[N:17]/[C:18]2[CH:27]=[CH:26][C:21]3[NH:22][C:23](=[S:25])[NH:24][C:20]=3[CH:19]=2)[C:13]2[O:30][CH2:28][O:16][C:14]=2[CH:15]=1

Komponenten

5

Edukt 4

HCID 176Acetic AcidHCID 3776IsopropanolHCID 27340026-Amino-2-mercaptobenzimidazoleHCID 110316405-Bromo-1,3-benzodioxole-4-carboxaldehyde

Produkt 1

HCID 178527899HCID 178527899, VerbindungAusbeute 83 %

Versuchsvorschrift

5-bromobenzo[d][1,3]dioxol-4-carbaldehyde (0.24 g, 1.05 mmol), IPA (4.8 ml), and 5-amino-1H-benzo[d]imidazole-2(3H)-thione (0.2 g, 1.21 mmol) were put in a 25 ml flask, and acetic acid (10 ml) was slowly added dropwise thereto while the mixture was stirred under nitrogen charging conditions, followed by stirring for 12 hours under reflux conditions. After that, the temperature of the mixture was lowered to room temperature, and the thus obtained solid was washed with methylene chloride and methanol, followed by filtering, thereby obtaining clean (E)-5-((6bromobenzo[d][1,3]dioxol-4-yl)methyleneamino)-1H-benzo[d]imidazole-2(3H)-thione at 83% yield.

Aufarbeitung

  1. stirringby stirring for 12 hours under reflux conditions
  2. customwas lowered to room temperature
  3. washthe thus obtained solid was washed with methylene chloride and methanol
  4. filtrationby filtering

Quellen und Nachweise

ORD-Eintrag
ord-4ae515f8bb65489f940b93c4b1570404
Quelldatensatz
uspto-grants-2016_04
Patentnummer
US09321751B2

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