HuagongsheHuagongshe Chemistry Print Report · For research reference only
HCID 22614896, compound → 5-Amino-6,7-dichloro-2,3-dimethoxyquinoxaline
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | HCID 22614896 | HCID 22614896 | — |
| Catalyst | Palladium | HCID 23938 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | 5-Amino-6,7-dichloro-2,3-dimethoxyquinoxaline | HCID 10606620 | 78.5% |
Reaction Steps
6,7-Dichloro-2,3-dimethoxy-5-nitroquinoxaline (20 g, 0.066 mol) and 5% w/w palladium-on-carbon (50% wet) (1.2 g) were suspended in a mixture of tetrahydrofuran (0.12 L) and ethyl acetate (0.12 L). The mixture was hydrogenated at 60° C. and 414 kPa (60 psi) for 22 hours, cooled, diluted with dichloromethane (0.48 L) and the catalyst removed by filtration through celite (trade mark) filter aid. The solution was concentrated under reduced pressure with the gradual addition of toluene. The mixture was then filtered and the solid was washed with toluene (20 ml) to give the title compound as a brown solid (14.2 g, 78%), m.p. 182-4° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06376490B1 |
| Source dataset | uspto-grants-2002_04 |
| ORD ID | ord-61df4a5765e142f98012c1f9ac80c9ee |
| Source note | uspto-grants-2002_04 |