HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 23503177, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Reactant | 2-Ethoxy-5-nitronicotinic acid | HCID 23503225 | — |
| Catalyst | Palladium | HCID 23938 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | HCID 23503177 | HCID 23503177 | 48% |
Reaction Steps
A solution of 2-ethoxy-5-nitronicotinic acid (12.0 g, 56.6 mmol, prepared by the method described in WO9954333) in a mixture of EtOH (150 ml), H2O (150 ml), NaHCO3 (4.80 g, 57.0 mmol) and 10% palladium on carbon (1.0 g) was hydrogenated at 60 psi and at 60° C. for 6 h. The mixture was cooled, filtered and acidified with AcOH. The mixture was concentrated in vacuo and the residue triturated with DCM/MeOH (95:5) to afford the title compound as a brown/purple solid (5.0 g, 27.5 mmol, 48%); mp 260-262° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06770645B2 |
| Source dataset | uspto-grants-2004_08 |
| ORD ID | ord-47f68a20b43b4070b46322245d8d94e4 |
| Source note | uspto-grants-2004_08 |