HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → 2-Amino-4-bromo-5-fluorobenzoic acid
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Hydrogen Peroxide | HCID 784 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | 6-Bromo-5-fluoroindoline-2,3-dione | HCID 67517039 | — |
| Product | 2-Amino-4-bromo-5-fluorobenzoic acid | HCID 67514961 | 25% |
Reaction Conditions
| Temperature | 0 °C |
|---|
Reaction Steps
To a 100 mL round bottom flask, 6-bromo-5-fluoro-1H-indole-2,3-dione (3 g, 0.0121 mol) and 2N NaOH (15 mL) were added and cooled the reaction vessel to 0° C. To this reaction mixture 30% hydrogen peroxide (10.5 mL) was slowly added. The reaction mixture was stirred at 0° C. for 3 h. Subsequently, the reaction mixture was acidified with 2 N HCl at 0° C. [pH-5] to afford the solid compound. The solid material was collected by filtration and dried to obtain the title compound (700 mg, 25%). 1H NMR (300 MHz, DMSO-d6): δ 7.52 (d, J=9.6 Hz, 1H), 7.09 (d, J=6.0 Hz, 1H); LC-MS (ESI): Calculated mass: 232.9; Observed mass: 231.9 [M−H]+ (RT: 0.23 min).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09115092B2 |
| Source dataset | uspto-grants-2015_08 |
| ORD ID | ord-a5da36e5b3ec4c68bfb546032b1a9df2 |
| Source note | uspto-grants-2015_08 |