Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Pyrrolidine | HCID 31268 | — |
| Reactant | 6-Cyanopyridine-3-carboxylic acid | HCID 2761108 | — |
| Reactant | 1,4-Dioxane hydrochloride | HCID 20443148 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | HCID 68594952 | HCID 68594952 | — |
Reaction Steps
6-Cyanonicotinic acid (4.15 g, 28.0 mmol) was dissolved in anhydrous ethanol (3.2 ml) and 4N hydrochloric acid/1,4-dioxane (30 ml), and the mixture was stirred in a closed system at room temperature for two nights. The solvent was evaporated under reduced pressure, and the obtained residue was suspended in anhydrous ethanol (90 ml). Pyrrolidine (2.34 ml, 28.0 mmol) was added thereto, and the mixture was stirred at room temperature for 3 days. Pyrrolidine (3.51 ml, 42.0 mmol) was added again, and the mixture was stirred for 2.5 hours. The solvent was evaporated under reduced pressure, and water aid ethanol were added to the obtained residue. The precipitate was removed by filtration, ethanol was evaporated under reduced pressure, and the obtained aqueous solution was lyophilized to give the title compound without purification operation.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08227506B2 |
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| Source dataset | uspto-grants-2012_07 |
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| ORD ID | ord-0e6c831969b9479dba4e46ae8bed3eb2 |
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| Source note | uspto-grants-2012_07 |
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