Methanesulfonic Acid → HCID 178493039, compound

To a solution of aminoguanidine hydrochloride (0.023 g) in ethanol (10 ml) was added methanesulfonic acid (0.02 g), and the mixture was refluxed for 30 minutes. To the solution was added 4-methoxy-7-phenyl-5,6,7,8-tetrahydroquinolin-5-one (0.05 g), and the mixture was stirred at room temperature for 2 hours and 20 minutes and at 50° C. for 25 minutes. To the mixture was added methanesulfonic acid (0.02 g), and the mixture was stirred at 50° C. for 5 hours. Under reduced pressure, the solvent was evaporated, and the residue was dissolved in water. The solution was washed with ethyl acetate. Under reduced pressure, the solvent was evaporated, and the residue was recrystallized from ethanol-water to give 5-guanidinoimino-4-methoxy-7-phenyl-5,6,7,8-tetrahydroquinoline methanesulfonate (Compound 78) (0.09 g) as colorless crystals.

1. temperaturethe mixture was refluxed for 30 minutes
2. stirringthe mixture was stirred at 50° C. for 5 hours
3. customUnder reduced pressure, the solvent was evaporated
4. dissolutionthe residue was dissolved in water
5. washThe solution was washed with ethyl acetate
6. customUnder reduced pressure, the solvent was evaporated
7. customthe residue was recrystallized from ethanol-water

ORD record

ord-1691a1fd8bb54385a7c14bdb37ac3354

Source dataset

uspto-grants-2002_02

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US06350749B1