Acetic Acid → HCID 20506357, Verbindung
Reaktionsgleichung
[NH2:1][C:2]1[CH:7]=[C:6]([Cl:8])[CH:5]=[CH:4][C:3]=1[NH:9][CH2:10][CH2:11][CH2:12][OH:13].Cl.[C:15](O)(=O)[CH3:16]>>[Cl:8][C:6]1[CH:5]=[CH:4][C:3]2[N:9]([CH2:10][CH2:11][CH2:12][OH:13])[C:15]([CH3:16])=[N:1][C:2]=2[CH:7]=1Komponenten
4
Versuchsvorschrift
A mixture of 20 parts of 3-[(2-amino-4-chlorophenyl)amino]-1-propanol, 50 parts of acetic acid and 150 parts of a hydrochloric acid solution 4 N is stirred and refluxed overnight. The reaction mixture is cooled and evaporated. The residue is dissolved in water and the solution is alkalized with ammonium hydroxide. The product is extracted with trichloromethane. The extract is dried, filtered and evaporated. The residue is crystallized from a mixture of 4-methyl-2-pentanone and 2,2'-oxybispropane, yielding 5-chloro-2-methyl-1H-benzimidazole-1-propanol.
Aufarbeitung
- temperaturerefluxed overnight
- temperatureThe reaction mixture is cooled
- customevaporated
- dissolutionThe residue is dissolved in water
- extractionThe product is extracted with trichloromethane
- customThe extract is dried
- filtrationfiltered
- customevaporated
- customThe residue is crystallized from a mixture of 4-methyl-2-pentanone and 2,2'-oxybispropane
Quellen und Nachweise
- ORD-Eintrag
- ord-b9ab71f281bf42c4a719ebede9504fab
- Quelldatensatz
- uspto-grants-1983_03
- Patentnummer
- US04377578
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