反应详情

To a solution of 7-(2-chlorophenyl)-4-trifluoromethyl-5,6,7,8-tetrahydrocinnolin-5-one (0.335 g) and aminoguanidine hydrochloride (165 mg) in ethanol (10 ml) were added methanesulfonic acid (0.3 ml) and benzene (10 ml), and the mixture was refluxed for 80 minutes. 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 acetone, and to the solution was added methanesulfonic acid (0.15 ml). Precipitated crystals were filtered, washed with acetone and dried to give 7-(2-chlorophenyl)-5-guanidinoimino-4-trifluoromethyl-5,6,7,8-tetrahydrocinnoline methanesulfonate (Compound 136) (0.240 g) as yellow crystals.

1. temperaturethe mixture was refluxed for 80 minutes
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 acetone
8. additionto the solution was added methanesulfonic acid (0.15 ml)
9. customPrecipitated crystals
10. filtrationwere filtered
11. washwashed with acetone
12. customdried