HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dimethylformamide → 5-Fluoro-2-nitrobenzamide
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dimethylformamide | HCID 6228 | — |
| Reactant | Ammonium Hydroxide | HCID 14923 | — |
| Reactant | Oxalyl chloride | HCID 65578 | — |
| Reactant | 5-Fluoro-2-nitrobenzoic acid | HCID 2737420 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | 5-Fluoro-2-nitrobenzamide | HCID 18668165 | 88% |
Reaction Steps
To 5-Fluoro-2-nitro-benzoic acid (3 g, 16.2 mmol) in 200 mL of methylene chloride was added oxalyl chloride (2.26 g, 17.8 mmol) and a drop of DMF. After stirring for 2 h, the solution was poured into concentrated NH4OH. The partial solution was poured into water, extracted with Ethyl acetate, dried (Na2SO4) and concentrated to give 5-Fluoro-2-nitro-benzamide (2.61 g, 88% yield) used without purification. LCMS m/e 185.1 (M+H) 183.2 (M-H), HPLC tr=2.9 min (100%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07842712B2 |
| Source dataset | uspto-grants-2010_11 |
| ORD ID | ord-165748cedf7e4997854e02a456cc80fc |
| Source note | uspto-grants-2010_11 |