Sulfuric Acid → 5-(3,4-dichlorophenyl)-2,3,5,6-tetrahydro-1H-imidazo[1,2-a]imidazole hydrochloride
Reaktionsgleichung
[Cl:1][C:2]1[CH:3]=[C:4]([CH:14]=[CH:15][C:16]=1[Cl:17])[CH:5](O)[CH2:6][NH:7][C:8]1[NH:9][CH2:10][CH2:11][N:12]=1.S(=O)(=O)(O)O.[OH-].[Na+]>>[ClH:1].[Cl:1][C:2]1[CH:3]=[C:4]([CH:5]2[N:12]3[CH2:11][CH2:10][NH:9][C:8]3=[N:7][CH2:6]2)[CH:14]=[CH:15][C:16]=1[Cl:17]Komponenten
4
Versuchsvorschrift
4.3 parts of 3,4-dichloro-α-(2-imidazolin-2-ylaminomethyl)benzyl alcohol are added portionwise to 16.2 parts of sulfuric acid solution 80% while stirring and cooling. Upon completion, the mixture is stirred for 2 hr. 30 min. at room temperature. The reaction mixture is poured onto ice-water, alkalized with concentrated sodium hydroxide solution and the product in base form is extracted with methylene chloride. The organic layer is dried, filtered and evaporated. The residue is converted into the hydrochloride salt in 2-propanol, yielding 5-(3,4-dichlorophenyl)-2,3,5,6-tetrahydro-1H-imidazo[1,2-a]imidazole hydrochloride; m.p. 298.4°C (dec.).
Aufarbeitung
- temperaturecooling
- stirringUpon completion, the mixture is stirred for 2 hr
- custom30 min.
- customat room temperature
- additionThe reaction mixture is poured onto ice-water
- extractionthe product in base form is extracted with methylene chloride
- customThe organic layer is dried
- filtrationfiltered
- customevaporated
Quellen und Nachweise
- ORD-Eintrag
- ord-ecced284432843a59edf1606cee6fd01
- Quelldatensatz
- uspto-grants-1976_06
- Patentnummer
- US03963718
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