HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sulfuric Acid → HCID 22097097, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sulfuric Acid | HCID 1118 | — |
| Reactant | HCID 22097137 | HCID 22097137 | — |
| Reactant | Sodium Nitrite | HCID 23668193 | — |
| Catalyst | HCID 178419072 | HCID 178419072 | — |
| Solvent | Acetic Acid | HCID 176 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | HCID 22097097 | HCID 22097097 | 64% |
Reaction Steps
14.2 g (57 mmol) of 6-amino-1-ethyl-7-nitro-2,3(1H,4H)-quinoxalinedione (Example 30a) were suspended in 340 ml of acetic acid. To this was added dropwise at 10°-20° C. a solution of 5.1 g (74 mmol) of sodium nitrite and 80 ml of concentrated sulfuric acid. The mixture was stirred for a further 30 minutes and then this solution was added dropwise to another suspension of 16.3 g (114 mmol) of copper(I) oxide in 140 ml ethanol. The mixture was stirred for a further 10 minutes and then poured into 11 of ice-water. After filtration, the filtrate was extracted with methylene chloride and the organic phase was dried and concentrated under reduced pressure to yield 8.5 g (64%) of the product. Melting point>300° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05714489 |
| Source dataset | uspto-grants-1998_02 |
| ORD ID | ord-ed0709cb7cbc48cdb76b81d608cc1ecd |
| Source note | uspto-grants-1998_02 |