Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Acetylacetone | HCID 31261 | — |
| Reactant | 2,6-Difluoroaniline | HCID 79647 | — |
| Reactant | Sodium Acetate | HCID 517045 | — |
| Reactant | Sodium Nitrite | HCID 23668193 | — |
| Solvent | Acetic Acid | HCID 176 | — |
| Solvent | Hydrochloric Acid | HCID 313 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 178468364 | HCID 178468364 | 21.5% |
Reaction Steps
To a solution of 2,6-difluoroaniline (1.0 g, 7.75 mmol) in 11.1 mL of acetic acid and 1.69 mL of concentrated hydrochloride solution, sodium nitrite (600 mg, 9.3 mmol) in 2.7 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 (1.78 g, 21.7 mmol) and acetylacetone (1 g, 10 mmol). 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 (400 mg, 21% yield): 1H NMR (400 MHz, CDCl3): δ ppm 2.43 (s, 3H), 2.61 (s, 3H), 6.97-7.03 (m, 2H), 7.05-7.15 (m, 1H), 14.42 (s, 1H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08916566B2 |
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| Source dataset | uspto-grants-2014_12 |
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| ORD ID | ord-4358b9ecfe674d23a7e027cda0f9581f |
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| Source note | uspto-grants-2014_12 |
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