Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Dimethylformamide | HCID 6228 | — |
| Reactant | Ammonium Chloride | HCID 25517 | — |
| Reactant | HCID 10538968 | HCID 10538968 | — |
| Reactant | Chloroform methanol | HCID 21584188 | — |
| Catalyst | Zinc | HCID 23994 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 10584029 | HCID 10584029 | 57.5% |
Reaction Steps
To a mixture of 6.2 g of 2-ethoxalylamino-4-fluoronitrobenzene and 124 ml of DMF was added a solution of 5.64 g of ammonium chloride in 40 ml of water. Then, 5.7 g of zinc dust was added in small portions to the above mixture. The reaction mixture was stirred under TLC (5% methanol-chloroform) monitoring and, when the starting material had disappeared, the mixture was filtered using Celite and washed with hot DMF. The mixture was heated at 100° C. for 3 hours, after which it was ice-cooled and the resulting inorganic salt crystals were filtered off. To the organic layer was added methanol and the resulting crystals were recovered by filtration to provide 2.73 g of 6-fluoro-1-hydroxyquinoxaline-2,3-(1H,4H)-dione.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US05283244 |
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| Source dataset | uspto-grants-1994_02 |
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| ORD ID | ord-063188e08e1a42b3be012b8d2eb29d0c |
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| Source note | uspto-grants-1994_02 |
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