Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | 2,3-Dichloropropiononitrile | HCID 92935 | — |
| Reactant | 4-Hydrazinopyridine | HCID 416631 | — |
| Solvent | Water | HCID 962 | — |
| Product | 1250155-26-0 | HCID 54078236 | 6% |
Reaction Steps
To a solution of potassium carbonate (4.46 g, 32 mmol) in water (20 ml) was added pyridine-4-yl-hydrazine×2HCl (1.47 g, 8 mmol) and the mixture was cooled to 10° C. 2,3-Dichloropropionitrile (1.0 g, 8 mmol) was added dropwise at that temperature. Subsequently, the mixture was stirred at 45° C. for 3 h and at ambient temperature overnight. The reaction mixture was extracted with dichloromethane, the organic phases were combined, washed with brine, dried and the solvent was evaporated. Silica gel chromatography using a heptane/ethyl acetate gradient yielded the amine as yellow solid (80 mg, 6%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08470820B2 |
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| Source dataset | uspto-grants-2013_06 |
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| ORD ID | ord-60c78080c7a744d1baa990622fc98c0d |
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| Source note | uspto-grants-2013_06 |
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