反应详情

A mixture of 6-(2-chlorophenyl)-3-phenylamino-4,5,6,7-tetrahydroindazol-4-one (0.4 g), aminoguanidine hydrochloride (0.16 g), concentrated hydrochloric acid (0.31 ml), water (0.31 ml) and ethanol (20 ml) was refluxed for 6 hours. Under reduced pressure, the solvent was evaporated, and to the residue was added sodium hydrogen carbonate solution to make the solution alkaline. The mixture was extracted with ethylacetate, and the organic layer was washed with water and concentrated under reduced pressure. The residue was dissolved in ethanol, and to the solution was added 1N hydrochloric acid (5 ml) and concentrated. Precipitated crystals were recrystallized from ethanol to give 6-(2-chlorophenyl)-4-guanidinoimino-3-phenylamino-4,5,6,7-tetrahydroindazole hydrochloride (Compound 146) (0.23 g) as colorless crystals.

1. temperaturewas refluxed for 6 hours
2. customUnder reduced pressure, the solvent was evaporated
3. additionto the residue was added sodium hydrogen carbonate solution
4. extractionThe mixture was extracted with ethylacetate
5. washthe organic layer was washed with water
6. concentrationconcentrated under reduced pressure
7. dissolutionThe residue was dissolved in ethanol
8. additionto the solution was added 1N hydrochloric acid (5 ml)
9. concentrationconcentrated
10. customPrecipitated crystals
11. customwere recrystallized from ethanol