HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 178468347, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Acetylacetone | HCID 31261 | — |
| Reactant | 2-Fluoro-5-(trifluoromethyl)aniline | HCID 136349 | — |
| Reactant | Potassium Acetate | HCID 517044 | — |
| Reactant | Sodium Nitrite | HCID 23668193 | — |
| Solvent | Acetic Acid | HCID 176 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 178468347 | HCID 178468347 | 64% |
Reaction Steps
2-Fluoro-5-(trifluoromethyl)aniline (2.00 g, 15.6 mmol) was added to a solution of 15.6 mL of HOAc and 2.6 mL of concentrated HCl, stirred, followed by sodium nitrite (0.925 g, 13.4 mmol) in 4 mL of water dropwise at 0° C., and the mixture was stirred at 0° C. for 60 min. Then potassium acetate (3.28 g, 3.5 mmol) and acetylacetone (1.83 mL, 14.5 mmol) were added dropwise. The mixture was stirred at room temperature overnight, filtered. The precipitate was dissolved in CH2Cl2, washed with water, dried over Na2SO4 and concentrated under reduced pressure to give the title compound (2.06 g, 64% yield): 1H NMR (400 MHz, CDCl3): δ ppm 2.53 (s, 3H), 2.64 (s, 3H), 7.26-6.30 (m, 1H), 7.39-7.42 (m, 1H), 7.99-8.01 (m, 1H), 14.62 (s, 1H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08916566B2 |
| Source dataset | uspto-grants-2014_12 |
| ORD ID | ord-09480b1e990247c794292c4751957af9 |
| Source note | uspto-grants-2014_12 |