HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triphenylphosphine → 1-[(Diethoxyphosphoryl)methyl]-7-trifluoromethyl[1,2,4]triazolo[4,3-a]quinoxalin-4(5H)-one
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triphenylphosphine | HCID 11776 | — |
| Reactant | 3-[2-[(Diethoxyphosphoryl)acetyl]hydrazino]-1-hydroxy-7-trifluoromethylquinoxalin-2(1H)-one | HCID 19421449 | — |
| Solvent | Acetic Acid | HCID 176 | — |
| Product | 1-[(Diethoxyphosphoryl)methyl]-7-trifluoromethyl[1,2,4]triazolo[4,3-a]quinoxalin-4(5H)-one | HCID 19421428 | 40% |
Reaction Steps
A solution of 3-[2-[(diethoxyphosphoryl)acetyl]hydrazino]-1-hydroxy-7-trifluoromethylquinoxalin-2(1H)-one (438 mg, 1 mmol) and triphenylphosphine (525 mg, 2 mmol) in 25 ml of glacial acetic acid was heated under reflux overnight (ca. 15 h). The mixture was evaporated to dryness, and the residue was flash chromatographed (SiO2) with dichloromethane to remove excess triphenylphosphine, then with ethyl acetate to remove triphenylphosphine oxide, and finally with 5% acetic acid in ethyl acetate to give 161 mg (40%) of the title compound. M.p. 224°-226° C., dec. (ethanol).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05559106 |
| Source dataset | uspto-grants-1996_09 |
| ORD ID | ord-c9e15b18de864f2cb7bc5edbd337cb50 |
| Source note | uspto-grants-1996_09 |