反应详情

(+)8,9-dihydro-10-methyl-7-[(5-methyl-1H-imidazol-4-yl)methyl]pyrido[1,2-a]indol-6(7H)-one (8.0 g) was dissolved in ethanol (80 ml) and water (72 ml), and 6 N hydrochloric acid (8 ml) was added thereto at an interior temperature of 20~30° C., and it was agitated at the same temperature for 1 hr. It was clarified by filtration, and the container and so forth was washed with ethanol (8 ml). Water (272 ml) was dripped therein at a temperature of 20~30° C. over the course of 20 min, and the seed crystals (0.016 g) were added thereto, and it was agitated at the same temperature for 3 hr, cooled to 0~5° C., and agitated for 3 hr. The precipitated crystals were collected by filtration, washed with water (32 ml), and thereafter 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·hydrochloride.

1. filtrationIt was clarified by filtration
2. washthe container and so forth was washed with ethanol (8 ml)
3. additionat a temperature of 20~30° C. over the course of 20 min, and the seed crystals (0.016 g) were added
4. stirringit was agitated at the same temperature for 3 hr
5. temperaturecooled to 0~5° C.
6. stirringagitated for 3 hr
7. filtrationThe precipitated crystals were collected by filtration
8. washwashed with water (32 ml)
9. customdried overnight under vacuum