Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | FK 1052 | HCID 125368 | — |
| Solvent | Ethanol | HCID 702 | — |
| Solvent | Water | HCID 962 | — |
| Product | FK1052 hydrochloride | HCID 9949384 | 82% |
Reaction Steps
(+)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.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US06013653 |
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| Source dataset | uspto-grants-2000_01 |
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| ORD ID | ord-0199ee6c34714cd0924102221ffb2177 |
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| Source note | uspto-grants-2000_01 |
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