反应详情

温度

35 °C

(±)8,9-dihydro-10-methyl-7-[(5-methyl-1H-imidazol-4-yl)methyl]pyrido[1,2-a]indol-6(7H)-one (100 g), (1R)-(-)-10-camphorsulfonic acid monohydrate (85.3 g), and radiolite (1 g) in ethanol (1,000 ml) were heated under reflux. It was cooled to 35° C., and 0.2 g of seed crystals were added thereto, thereafter it was agitated at an interior temperature of 20~30° C. for 3 hr, and after ethanol (1,000 ml) was added therto, it was agitated overnight at 20~30° C. The following day, water (25 ml) was added thereto and it was agitated for 1 hr at 20~30° C., and after the temperature was raised to 33~37° C., it was agitated for 30 min. It was cooled to 20~30° C., thereafter the precipitated crystals were collected by filtration, washed with ethanol (100 ml), and dried overnight under vacuum to obtain (+)8,9-dihydro-10-methyl-7-[(5-methyl-1H-imidazol-4-yl)methyl]pyrido[1,2-a]indol-6(7H)-one·CSA salt as colorless coarse crystals.

1. temperatureunder reflux
2. addition0.2 g of seed crystals were added
3. stirringwas agitated overnight at 20~30° C
4. stirringit was agitated for 1 hr at 20~30° C.
5. temperatureafter the temperature was raised to 33~37° C.
6. stirringit was agitated for 30 min
7. temperatureIt was cooled to 20~30° C.
8. filtrationthe precipitated crystals were collected by filtration
9. washwashed with ethanol (100 ml)
10. customdried overnight under vacuum