反应详情

To 80 parts thionylchloride (previously cooled to 0°C.) are added 10.15 parts 2-(β-hydroxy-phenethyl-amino)-2-imidazoline. After the addition is complete, the whole is stirred for 30 minutes at room temperature and further stirred and refluxed for 15 minutes. The solvent is evaporated. The residue is dissolved in 40 parts toluene and evaporated again. This treatment is repeated by using 40 parts methanol. The residue is then dissolved in 40 parts 2-propanol. To this solution is added a solution of 1.15 parts sodium metal in 40 parts 2-propanol. The whole is stirred and refluxed for one hour. The solvent is evaporated. The residue is dissolved in 150 parts water. The solution is filtered. The filtrate is alkalized with ammonium hydroxide and extracted three times with 40 parts ether and three times with 75 parts chloroform. The combined extracts are dried over potassium carbonate and evaporated. The solid residue is recrystallized from a mixture of 16 parts acetone and 16 parts 4-methyl-2-pentanone, yielding 2,3,5,6-tetrahydro-5-phenyl-1H-imidazo[1,2-a]imidazole; m.p. 167°-169.5°C.

1. additionAfter the addition
2. stirringfurther stirred
3. temperaturerefluxed for 15 minutes
4. customThe solvent is evaporated
5. dissolutionThe residue is dissolved in 40 parts toluene
6. customevaporated again
7. dissolutionThe residue is then dissolved in 40 parts 2-propanol
8. additionTo this solution is added a solution of 1.15 parts sodium metal in 40 parts 2-propanol
9. stirringThe whole is stirred
10. temperaturerefluxed for one hour
11. customThe solvent is evaporated
12. dissolutionThe residue is dissolved in 150 parts water
13. filtrationThe solution is filtered
14. extractionextracted three times with 40 parts ether and three times with 75 parts chloroform
15. dry with materialThe combined extracts are dried over potassium carbonate
16. customevaporated
17. customThe solid residue is recrystallized from a mixture of 16 parts acetone and 16 parts 4-methyl-2-pentanone