HuagongsheHuagongshe Chemistry Print Report · For research reference only
Picolinic acid → HCID 2771595, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Picolinic acid | HCID 1018 | — |
| Reactant | 1-Hydroxybenzotriazole | HCID 75771 | — |
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Reactant | Ethyl 2-amino-2-cyanoacetate | HCID 288716 | — |
| Reactant | 1,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochloride | HCID 2723939 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 2771595 | HCID 2771595 | 30% |
Reaction Steps
To a solution of picolinic acid (1.23 g, 10 mmol), EDC.HCl (1.91 g, 10 mmol) and HOBT (1.35 g, 10 mmol) in THF (80 mL) was added DIPEA (3.6 g, 30 mmol) at ambient temperature. The reaction mixture was maintained at the same temperature for 1 hr at which time a solution of ethyl 2-amino-2-cyanoacetate (1.28 g, 10 mmol) in THF (5 mL) was added. The reaction mixture was stirred at ambient temperature for additional 6 hr. It was then concentrated, and the residue was purified by silica gel column chromatography (5:1 PE/EtOAc) to give ethyl 2-cyano-2-(picolinamido)acetate (0.7 g, 30%) as yellow solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09328106B2 |
| Source dataset | uspto-grants-2016_05 |
| ORD ID | ord-604a8e8f4a4640b0a14f5be0b4bc902d |
| Source note | uspto-grants-2016_05 |