反应详情

To 400 ml of N-methylpyrrolidone, 144.4 g (0.6 mol) of 1-chloro-4-phenylphthalazine and 230 g (1.8 mol) of (R)-(-)-1-cyclohexylethylamine were added, and the mixture was heated to 120° to 130° C. for 6 hours with stirring. After completion of the reaction, the mixture was cooled and added with 4.0 l of 5% aqueous NaOH solution, and then extracted with chloroform. The organic layer was dried over MgSO4, concentrated and purified by silica gel column chromatography (eluent; ethyl acetate/hexane/chloroform=1:3:1). After recrystallization from ether/chloroform, 150.2 g of (R)-1-(1-cyclohexylethylamino)-4-phenylphthalazine was obtained. m.p. 164.0°-167.0° C.

1. temperaturethe mixture was heated to 120° to 130° C. for 6 hours
2. customAfter completion of the reaction
3. temperaturethe mixture was cooled
4. extractionextracted with chloroform
5. dry with materialThe organic layer was dried over MgSO4
6. concentrationconcentrated
7. custompurified by silica gel column chromatography (eluent; ethyl acetate/hexane/chloroform=1:3:1)
8. customAfter recrystallization from ether/chloroform