Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Pyridine | HCID 1049 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | 4-(Aminomethyl)Benzoic Acid | HCID 65526 | — |
| Reactant | HCID 66893771 | HCID 66893771 | — |
| Catalyst | 4-(Dimethylamino)pyridine | HCID 14284 | — |
| Product | HCID 66894164 | HCID 66894164 | 44% |
Reaction Steps
To a mixture of 3-methylsulfanyl-3-(pyridin-4-ylamino)-acrylonitrile (0.2 g, 1.0 mmol), 4-aminomethyl-benzoic acid (0.173 g, 1.14 mmol), DMAP (1 mg) and Et3N (0.14 ml, 1.0 mmol) was added dry pyridine (0.5 ml). The resulting stirring mixture was heated to 55° C. for 4.5 hrs., additional Et3N (0.14 ml) was added and mixture was heated from 75° C. to 90° C. over a period of ˜30 hrs. When the reaction was complete, pyridine was partially removed in vacuo and the crude was purified by column chromatography (gradient of EtOAc to 20% MeOH/EtOAc) to afford the desired product as an off-white solid (130 mg, 44%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07595343B2 |
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| Source dataset | uspto-grants-2009_09 |
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| ORD ID | ord-47b9e130b3d54bdf9eddf6bfabf4e74e |
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| Source note | uspto-grants-2009_09 |
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