HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 136092327, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | Boron tribromide | HCID 25134 | — |
| Reactant | HCID 21189996 | HCID 21189996 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 136092327 | HCID 136092327 | 88.5% |
Reaction Steps
To a suspension of 6,7-dimethoxy-2,3-quinoxalinedione (45) (222 mg, 1.0 mmol) in 2 mL of methylene dichloride was added 5 mL of a solution of boron tribromide in methylene dichloride (1M, Aldrich). The resulting mixture was stirred at room temperature for 24 hr. The mixture was then poured into ice-water (10 g) to form a suspension. Aquous sodium hydroxide (20%, 10 mL) was added to the suspension to form a red solution. The solution was acidified with 6N HCl (10 mL) to pH=1. The suspension was centrifuged, washed with methanol, and dried in vacuo, giving 170 mg (88%) of the product as a brown solid; mp>350° C.; 1H NMR (DMSO-d6, 300 MHz) δ6.541 (s, 2H), 8.989 (s, 2H), 11.543 (s, 2H). EIMS m/e 194 (100, M+). (HPLC>99%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05631373 |
| Source dataset | uspto-grants-1997_05 |
| ORD ID | ord-824e083e88e1451d809db0bda97f1706 |
| Source note | uspto-grants-1997_05 |