反应详情

A mixture of 1,3-dimethyl-6-phenyl-4,5,6,7-tetrahydroindol-4-one (0.31 g), aminoguanidine hydrochloride (0.15 g), concentrated hydrochloric acid (0.065 ml), water (0.065 ml) and ethanol (50 ml) was refluxed for 5 hours. Under reduced pressure, the solvent was evaporated, and the residue was dissolved in water. The solution was washed with diethylether, and to the mixture was added sodium hydrogen carbonate solution. The mixture was extracted with ethyl acetate, and the organic layer was dried with magnesium sulfate. Under reduced pressure, the solvent was evaporated, and the residue was dissolved in ethanol. To the solution was added 1N hydrochloric acid. The solvent was evaporated, and the residue was recrystallized from ethanol-ethyl acetate to give 4-guanidinoimino-1,3-dimethyl-6-phenyl-4,5,6,7-tetrahydroindole hydrochloride (Compound 8) (0.1 g) as colorless crystals.

1. temperaturewas refluxed for 5 hours
2. customUnder reduced pressure, the solvent was evaporated
3. dissolutionthe residue was dissolved in water
4. washThe solution was washed with diethylether
5. additionto the mixture was added sodium hydrogen carbonate solution
6. extractionThe mixture was extracted with ethyl acetate
7. dry with materialthe organic layer was dried with magnesium sulfate
8. customUnder reduced pressure, the solvent was evaporated
9. dissolutionthe residue was dissolved in ethanol
10. additionTo the solution was added 1N hydrochloric acid
11. customThe solvent was evaporated
12. customthe residue was recrystallized from ethanol-ethyl acetate