反应详情

A mixture of 6-(2-chlorophenyl)-3-methoxymethyl-4,5,6,7-tetrahydroindazol-4-one (0.1 g), aminoguanidine hydrochloride (0.046 g), concentrated hydrochloric acid (0.086 ml), water (0.086 ml) and ethanol (10 ml) was refluxed for 5 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 ethyl acetate, and the organic layer was washed with water and concentrated under reduced pressure. The residue was dissolved in 1N hydrochloric acid (1ml), and the solution was concentrated. The resulting crystals were recrystallized from ethanol-ethyl acetate to give 6-(2-chlorophenyl)-4-guanidinoimino-3-methoxymethyl-4,5,6,7-tetrahydroindazole hydrochloride (Compound 148) (0.06 g) as colorless crystals.

1. temperaturewas refluxed for 5 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 ethyl acetate
5. washthe organic layer was washed with water
6. concentrationconcentrated under reduced pressure
7. dissolutionThe residue was dissolved in 1N hydrochloric acid (1ml)
8. concentrationthe solution was concentrated
9. customThe resulting crystals were recrystallized from ethanol-ethyl acetate