HuagongsheHuagongshe Chemistry Print Report · For research reference only
Nitric Acid → 4,5-Difluoro-2-nitrobenzoic acid
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Nitric Acid | HCID 944 | — |
| Reactant | 3,4-Difluorobenzoic acid | HCID 99166 | — |
| Reactant | Difluprednate | HCID 443936 | — |
| Solvent | Sulfuric Acid | HCID 1118 | — |
| Product | 4,5-Difluoro-2-nitrobenzoic acid | HCID 4219630 | 77.4% |
Reaction Conditions
| Temperature | 0 °C |
|---|
Reaction Steps
Into 100 mL of 96% sulfuric acid was placed 3,4-difluorobenzoic acid(11.95 g, 0.0756 mol). The solution was stirred at room temperature until the DFBA was dissolved, and then cooled to 0° C. Nitric acid (7.9 g of 90% fuming) was added dropwise to the cooled mixture. After addition, the solution was warmed to room temperature and stirred until completion of the reaction. After drying, 11.88 g of 2-nitro-4,5-difluorobenzoic acid was isolated. The material was identified by GCMS and 19F NMR analysis. An additional 2.41 g of product was obtained by extraction of the acid washes and removal of the solvent.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05003103 |
| Source dataset | uspto-grants-1991_03 |
| ORD ID | ord-c48e92e255584abb9fa0110bf70f4c79 |
| Source note | uspto-grants-1991_03 |