HuagongsheHuagongshe Chemistry Print Report · For research reference only
5-Bromo-8-(3,5-dimethoxy-phenyl)-quinoxaline → 8-(3,5-Dimethoxy-phenyl)-quinoxaline-5-carbonitrile
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 5-Bromo-8-(3,5-dimethoxy-phenyl)-quinoxaline | HCID 59292825 | — |
| Reactant | HCID 178418546 | HCID 178418546 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Solvent | N-methyl-2-pyrrolidone | HCID 13387 | — |
| Product | 8-(3,5-Dimethoxy-phenyl)-quinoxaline-5-carbonitrile | HCID 59292884 | — |
Reaction Conditions
| Temperature | 180 °C |
|---|
Reaction Steps
A mixture of 5-bromo-8-(3,5-dimethoxy-phenyl)-quinoxaline (Step 1.4) (4.54 g, 13.2 mmol) and CuCN (1.54 g, 17.1 mmol, 1.3 equiv) in NMP (50 mL) was stirred for 2 h at 180° C., under an argon atmosphere. The reaction mixture was allowed to cool to rt, diluted with EtOAc (10% aqueous solution of ethylenediamine) (150 mL), and filtered to afford 1.19 g (batch 1) of the title compound as a yellow solid. The filtrate was extracted with DCM. The organic phase was washed with H2O and brine, dried (Na2SO4), filtered and concentrated. The residue was triturated in EtOAc to provide 2.31 g (batch 2) of the title compound: ESI-MS: 292.1 [M+H]+; tR=4.53 min (System 1).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08674099B2 |
| Source dataset | uspto-grants-2014_03 |
| ORD ID | ord-c45d212e0aea4ed887037ef6bcf0a301 |
| Source note | uspto-grants-2014_03 |