반응 #1464816

반응 방정식

2-(4-methylphenyl)-3-oxo-butyronitrile

ethanol

2,2-diethoxyethylhydrazine

hydrogen chloride

→

title compound

수율 72.3%

7-(4-Methylphenyl)-6-methyl-1H-imidazo[1,2-b]pyrazole

수율 72.3%

용매

diethyl ether

dioxane

반응 조건

후처리

1. 1
   온도was heated
2. 2
   온도under reflux for 7 hours
3. 3
   온도the whole mixture was heated
4. 4
   온도under reflux for a further 30 minutes
5. 5
   온도After the mixture had been cooled
6. 6
   기타to precipitate crystals
7. 7
   여과These were collected by filtration
8. 8
   기타partitioned between ethyl acetate and dilute aqueous ammonia
9. 9
   기타The organic phase was separated
10. 10
    세척washed with water
11. 11
    건조dried over anhydrous magnesium sulfate
12. 12
    기타The solvent was then removed by distillation under reduced pressure
13. 13
    기타to leave a residue, which
14. 14
    기타was recrystallized from a mixture of ethyl acetate and hexane

실험 절차

A mixture of 1.7 g of 2-(4-methylphenyl)-3-oxo-butyronitrile, 20 ml of ethanol and 1.5 g of 2,2-diethoxyethylhydrazine was heated under reflux for 7 hours. At the end of this time, 30 ml of 4N hydrogen chloride in dioxane were added, and then the whole mixture was heated under reflux for a further 30 minutes. After the mixture had been cooled, diethyl ether was added to precipitate crystals. These were collected by filtration and partitioned between ethyl acetate and dilute aqueous ammonia. The organic phase was separated, washed with water and dried over anhydrous magnesium sulfate. The solvent was then removed by distillation under reduced pressure, to leave a residue, which was recrystallized from a mixture of ethyl acetate and hexane, to give 1.5 g of the title compound. The physical and chemical properties of this compound were the same as those of the compound prepared as described in Example 36.

출처