HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ammonium Acetate → 2-Amino-4-fluoro-5-iodo-3-methoxy-6-methylbenzamide
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ammonium Acetate | HCID 517165 | — |
| Reactant | 7-Fluoro-6-iodo-8-methoxy-5-methyl-1H-benzo[d][1,3]oxazine-2,4-dione | HCID 86630806 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | 2-Amino-4-fluoro-5-iodo-3-methoxy-6-methylbenzamide | HCID 86097420 | 96.2% |
Reaction Steps
Under nitrogen atmosphere, ammonium acetate (4.62 g, 60.0 mmol) was added to an N,N-dimethylformamide (120 ml) solution of 7-fluoro-6-iodo-8-methoxy-5-methyl-1H-benzo[d][1,3]oxazine-2,4-dione (I-31) (4.2 g, 12.0 mmol), followed by stirring at room temperature for 16 hours. The reaction liquid was concentrated under reduced pressure, the residue was dissolved in ethyl acetate, washed three times with saturated brine, then dried over anhydrous magnesium sulfate. After filtration and concentration under reduced pressure, the resulting residue was suspended in diisopropyl ether, followed by filtration and drying to obtain the entitled compound (3.74 g, 96%) as a white solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07737166B2 |
| Source dataset | uspto-grants-2010_06 |
| ORD ID | ord-6c3079e911ed4d9c859525c4f48c18e5 |
| Source note | uspto-grants-2010_06 |