Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Methanesulfonic Acid | HCID 6395 | — |
| Reactant | Lurosetron | HCID 172999 | — |
| Solvent | 1-Propanol | HCID 1031 | — |
| Product | HCID 19044694 | HCID 19044694 | — |
Reaction Steps
Water (0.29 l) and methanesulphonic acid (0.23 l) was added to a suspension of 6-fluoro-2,3,4,5-tetrahydro-5-methyl-2-[(5-methyl-1H-imidazol-4-yl)methyl]-1H-pyrido[4,3-b]indol-1-one (1.04 kg) in propan-1-ol (7.4 l). The mixture was heated to about 65° C. to give a clear solution, which was filtered, and the filter rinsed with propan-1-ol. The combined filtrate and wash were cooled to about 15° C. and diisopropyl ether (7.9 l) was added to the resulting suspension. The mixture was cooled to 5° C., and the solid isolated by filtration, washed with diisopropyl ether:propan-1-ol (3:1, 2×1.8 l) and diisopropyl ether (2×2 l) and finally dried in vacuo at about 35° C. to yield the title compound (1.39 kg).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US05635513 |
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| Source dataset | uspto-grants-1997_06 |
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| ORD ID | ord-72bb633e86004fb6a91d31fe919028c7 |
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| Source note | uspto-grants-1997_06 |
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