反应详情

3.4 parts of p-chloro-α-(2-imidazoline-2-ylaminomethyl)benzyl alcohol are added to 30 parts of sulfuric acid 80% while stirring and cooling in an ice-bath. Upon completion, the whole is stirred for 2 hours at room temperature. The reaction mixture is poured onto crushed ice, alkalized with a concentrated sodium hydroxide solution and the product in base form is extracted with methylene chloride. The extract is dried, filtered and evaporated. The residue is dissolved in 2-propanol. The solution is filtered over diatomaceous silica and the filtrate is acidified with an excess of 2-propanol previously saturated with gaseous hydrogen chloride. The precipitated salt is filtered off, washed with acetone and dried, yielding 5-p-chlorophenyl)-2,3,5,6-tetrahydro-1H-imidazo[1,2-a]imidazole hydrochloride, m.p. 266.1°C.

1. temperaturecooling in an ice-bath
2. stirringUpon completion, the whole is stirred for 2 hours at room temperature
3. additionThe reaction mixture is poured
4. customonto crushed ice
5. extractionthe product in base form is extracted with methylene chloride
6. customThe extract is dried
7. filtrationfiltered
8. customevaporated
9. dissolutionThe residue is dissolved in 2-propanol
10. filtrationThe solution is filtered over diatomaceous silica
11. filtrationThe precipitated salt is filtered off
12. washwashed with acetone
13. customdried