HuagongsheHuagongshe Chemistry Print Report · For research reference only
Oxalic Acid → 6-Bromo-8-methyl-1,4,7,8,9,10-hexahydro-pyrido[4,3-f]quinoxaline-2,3-dione
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Oxalic Acid | HCID 971 | — |
| Reactant | 8-Bromo-1,2,3,4-tetrahydro-2-methyl-5,6-isoquinolinediamine | HCID 10355032 | — |
| Solvent | Hydrochloric Acid | HCID 313 | — |
| Product | 6-Bromo-8-methyl-1,4,7,8,9,10-hexahydro-pyrido[4,3-f]quinoxaline-2,3-dione | HCID 9818134 | 24.1% |
Reaction Steps
A solution of the product from Example 13 (0.62 g, 2.56 mmol) and oxalic acid (0.23 g, 2.56 mmol) in 25 mL of 3N aqueous HCl solution were heated at reflux for 18 hours. The reaction mixture was cooled to room temperature and the solid which formed was collected by filtration and washed with cold water. The solid was recrystallized from hot water and dried under vacuum (100° C., P2O5) to give the title compound as a tan solid (0.191 g, 20%), mp=315-320° C. (dec.).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06703391B2 |
| Source dataset | uspto-grants-2004_03 |
| ORD ID | ord-28485785eeb5490989bcf2076b9474c3 |
| Source note | uspto-grants-2004_03 |