Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Nitromethane | HCID 6375 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | HCID 18958067 | HCID 18958067 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 18958063 | HCID 18958063 | 86.5% |
Reaction Steps
60% Sodium hydride (3.0 g) was suspended in 20 ml of N,N-dimethylformamide, then 8.4 g of nitro-methane was gradually dropped thereinto with ice-cooling and stirring and the mixture was stirred at room temperature for 30 minutes. 2-Fluoro-5-methanesulfonylaminobenzoic acid (8.0 g) and 6.7 g of N,N'-carbonyldiimidazole were dissolved in 30 ml of N,N-dimethylformamide and the solution was made to react at room temperature for 1 hour. The reaction mixture was added, with ice-cooling, to the solution obtained hereinbefore and the mixture was stirred at room temperature for 2 hours. Then, the mixture was poured into ice water, acidified with hydrochloric acid and the crystals separated out therefrom were filtered, washed with small amount of ethanol and dried to give 8.2 g of 4'-fluoro-3'-(2-nitroacetyl)-methanesulfonanilide, m.p. 174°-176 ° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patent number | US05360822 |
|---|
| Source dataset | uspto-grants-1994_11 |
|---|
| ORD ID | ord-4082896c27f640a8825d37041e607ef8 |
|---|
| Source note | uspto-grants-1994_11 |
|---|