Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Acetylacetone | HCID 31261 | — |
| Reactant | Sodium Acetate | HCID 517045 | — |
| Reactant | 2-Fluoro-4-(trifluoromethyl)aniline | HCID 2737674 | — |
| Reactant | Sodium Nitrite | HCID 23668193 | — |
| Solvent | Acetic Acid | HCID 176 | — |
| Solvent | Hydrochloric Acid | HCID 313 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 178468336 | HCID 178468336 | 44.5% |
Reaction Steps
To a solution of 2-fluoro-4-(trifluoromethyl)aniline (1.0 g, 5.58 mmol) in 8 mL of acetic acid and 1.3 mL of concentrated hydrochloride solution, sodium nitrite (462 mg, 6.69 mmol) in 2.1 mL of water was added dropwise at 0° C., and the mixture was stirred at 0° C. for 1 h. Then to the reaction mixture were added sodium acetate (1.37 g, 16.8 mmol, 3.0 equiv.) and acetylacetone (726 mg, 7.26 mmol, 1.3 equiv.) The mixture was stirred at room temperature for 2 h, filtered, washed with water, EtOH/H2O (1/1) and hexane, and dried to give the title compound (720 mg, yield 44%): 1H NMR (400 MHz, CDCl3): δ ppm 2.51 (s, 3H), 2.63 (s, 3H), 7.42-7.50 (m, 2H), 7.86 (t, J=8.0 Hz, 1H), 14.56 (s, 1H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08435995B2 |
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| Source dataset | uspto-grants-2013_05 |
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| ORD ID | ord-6549dcd8fd58477d8d29fbb845bf57ca |
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| Source note | uspto-grants-2013_05 |
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