Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | 4-Aminopyridine | HCID 1727 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | 2-Propenenitrile, 3,3-bis(methylthio)- | HCID 5325445 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 66893771 | HCID 66893771 | 90.3% |
Reaction Steps
To a solution of pyridin-4-ylamine (1.0 g, 11.0 mmol) and 3,3-Bis-methylsulfanyl-acrylonitrile (2.05 g, 12.6 mmol) in DMF at room temperature, was added powdered 4 A molecular sieves. The mixture was stirred for 1 hr. Subsequently the mixture was cooled to 0° C., 60% NaH dispersion in oil (0.92 g, 23.0 mmol) was added portionwise over 1 hr. and it was stirred at 0° C. for an additional 2 hrs. The cold bath was removed and the mixture was stirred at room temperature for 20 hrs. DMF was removed in vacuo and the crude was purified by column chromatography (gradient of EtOAc to 25% MeOH/EtOAc) to afford the desired product as an off-white solid (1.9 g, 89%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07838520B2 |
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| Source dataset | uspto-grants-2010_11 |
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| ORD ID | ord-17a558ce781645dfb4399ecda90d8718 |
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| Source note | uspto-grants-2010_11 |
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