HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 22917216, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Barium Carbonate | HCID 10563 | — |
| Reactant | HCID 12283437 | HCID 12283437 | — |
| Reactant | HCID 178418361 | HCID 178418361 | — |
| Catalyst | Palladium Chloride | HCID 24290 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | HCID 22917216 | HCID 22917216 | — |
Reaction Steps
3-Chloro-6,7-dimethyl-2-quinoxalinecarboxylic acid, ethyl ester (Example 14a) (6.0 g), palladium chloride (0.4 g) and barium carbonate (17.4 g) in ethanol (500 ml) containing water (6 ml) were stirred in an atmosphere of hydrogen at room temperature and atmospheric pressure for 18 hours. The mixture was filtered and the filtrate was evaporated. The residue was crystallised from a mixture of ethyl acetate and light petroleum (b.p. 60°-80°). The solid was dissolved in aqueous sodium hydroxide (20 ml., 2N) and ethanol (20 ml) and the solution was heated under reflux for 10 minutes and cooled. Hydrochloric acid was added and the solid was collected and crystallised from aqueous ethanol. It had m.p. 214.5°-216° (20%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US03997535 |
| Source dataset | uspto-grants-1976_12 |
| ORD ID | ord-3e73a5f2533c4b9183636f56304be4b7 |
| Source note | uspto-grants-1976_12 |