反应详情

722 mg (3.0 mmol) of 1-chloro-4-phenylphthalazine and 1.15 g (9.0 mmol) of (R)-(-)-1-cyclohexylethylamine were added to 2 ml of N-methylpyrrolidone, and the resultant mixture was stirred at 120° to 130° C. for 6 hours under heating. After the end of the reaction, the mixture was cooled. 20 ml of an aqueous 5% NaOH solution was added to the mixture and the solution was extracted with chloroform. The organic layer was dried over MgSO4, concentrated, purified by silica gel chromatography (eluent: ethyl acetate:hexane:chloroform=1:3:1) and recrystallized from ether-chloroform, thereby obtaining 751 mg of (R)-1-(1-cyclohexylethylamino)-4-phenylphthalazine.

1. temperatureunder heating
2. customAfter the end of the reaction
3. temperaturethe mixture was cooled
4. extractionthe solution was extracted with chloroform
5. dry with materialThe organic layer was dried over MgSO4
6. concentrationconcentrated
7. custompurified by silica gel chromatography (eluent: ethyl acetate:hexane:chloroform=1:3:1)
8. customrecrystallized from ether-chloroform