HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium Iodide → 6-Bromo-1,2,3,4-tetrahydroquinoxalin-2-one
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium Iodide | HCID 5238 | — |
| Reactant | Sodium Carbonate | HCID 10340 | — |
| Reactant | N-(2-Amino-4-bromophenyl)-2-chloroacetamide | HCID 66911433 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | 6-Bromo-1,2,3,4-tetrahydroquinoxalin-2-one | HCID 66911307 | 34.1% |
Reaction Steps
A mixture of N-(2-amino-4-bromophenyl)-2-chloroacetamide (4.5 g, 17.0 mmol), sodium iodide (101 mg, 2.0 mmol) and sodium carbonate (3.6 g, 33.8 mmol) in 300 ml acetonitrile was refluxed overnight under an atmosphere of nitrogen. Then the acetonitrile was removed under vacuum. The resulting solid was suspended in 150 ml water acidified to pH 5-6 with 1 N HCl. Extraction with ethyl acetate, washing of the combined organic layers with brine, drying over MgSO4, removing the solvent under reduced pressure and purification of the crude product by flash chromatography on silica gel (petroleum ether/ethyl acetate, 1.5/1) yielded 6-bromo-3,4-dihydroquinoxalin-2(1H)-one (1.3 g, 5.8 mmol, 34%) as yellow solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08685960B2 |
| Source dataset | uspto-grants-2014_04 |
| ORD ID | ord-7d2690bd66654f5d9754c1f6d1021483 |
| Source note | uspto-grants-2014_04 |