Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Acetonitrile | HCID 6342 | — |
| Reactant | Acetonitrile--water (1/1) | HCID 18373917 | — |
| Reactant | 1488325-95-6 | HCID 131733699 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 131733698 | HCID 131733698 | — |
Reaction Steps
To a mixture of 598 g (0.99 mol) of (S)—N-((3S,5S,6R)-6-methyl-2-oxo-5-phenyl-1-(2,2,2-trifluoroethyl)piperidine-3-yl)-2′-oxo-1′,2′,5,7-tetrahydrospiro[cyclopenta[b]pyridine-6,3′-pyrrolo[2,3-b]pyridine]-3-carboxamide trihydrate and 3.2 L of acetonitrile was added 0.8 L of water. The mixture was heated to 30° C. to dissolve all solids. The solution was cooled to 20° C. and 6 g of acetonitrile/water solvate seeds was introduced. After the mixture was stirred at 20° C. 30 minutes, 4 L of water was added slowly over 4 hours. During the addition of water solids precipitated as acetonitrile/water mixed solvate.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US09174989B2 |
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| Source dataset | uspto-grants-2015_11 |
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| ORD ID | ord-6a5c889c1b8a427690ace87926659c89 |
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| Source note | uspto-grants-2015_11 |
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