HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydroxylamine HCl → 1-Ethoxycarbonylmethyl-7-(3-hydroxyiminomethyl-1-pyrrolyl)-6-trifluoromethyl-2,3(1H,4H)-quinoxalinedione
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydroxylamine HCl | HCID 21645 | — |
| Reactant | Sodium Acetate | HCID 517045 | — |
| Reactant | 1-(Ethoxycarbonylmethyl)-7-(3-formyl-1-pyrrolyl)-6-trifluoromethyl-2,3(1H,4H)-quinoxalinedione | HCID 15337997 | — |
| Solvent | Water ethanol | HCID 19096565 | — |
| Product | 1-Ethoxycarbonylmethyl-7-(3-hydroxyiminomethyl-1-pyrrolyl)-6-trifluoromethyl-2,3(1H,4H)-quinoxalinedione | HCID 54279603 | 130% |
Reaction Steps
1.2 g (2.9 mmol) of the compound from Example 70, 0.4 g (6 mmol) of hydroxylammonium chloride and 0.48 g (6 mmol) of sodium acetate in 45 ml of H2O/EtOH (2:1) were refluxed for 30 minutes. The organic solvent was removed under reduced pressure, and the resulting aqueous phase was extracted with ethyl acetate. The organic phase was dried and concentrated under reduced pressure. The residue was recrystallized from ethanol to yield 1.6 g (70%) of the product. Melting point>250° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05714489 |
| Source dataset | uspto-grants-1998_02 |
| ORD ID | ord-c9d1eb70d9964197984294fb12357841 |
| Source note | uspto-grants-1998_02 |