HuagongsheHuagongshe Chemistry Print Report · For research reference only
1,1,1,3,3,3-Hexafluoro-2-(3-nitrophenyl)propan-2-ol → 2-(3-Aminophenyl)-1,1,1,3,3,3-hexafluoropropan-2-ol
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 1,1,1,3,3,3-Hexafluoro-2-(3-nitrophenyl)propan-2-ol | HCID 279582 | — |
| Reactant | Ammonium formate | HCID 2723923 | — |
| Catalyst | Palladium | HCID 23938 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | 2-(3-Aminophenyl)-1,1,1,3,3,3-hexafluoropropan-2-ol | HCID 13320609 | 75.3% |
Reaction Steps
To a solution of 1,1,1,3,3,3-hexafluoro-2-(3-nitrophenyl)propan-2-ol (6.0 g, 21 mmol) in ethanol (60 mL) was added ammonium formate (6.0 g) and Pd/C (10%, 600 mg). The mixture was heated at reflux for 5 min and was cooled to room temperature. The Pd catalyst was removed via filtration through Celite using ethanol. The combined filtrate was evaporated to dryness and the residue was washed with CH2Cl2 to yield 2-(3-aminophenyl)-1,1,1,3,3,3-hexafluoropropan-2-ol (4.1 g, 67% over two steps). 1H NMR (400 MHz, DMSO-d6) δ 8.37 (s, 1H), 7.11 (t, J=7.9 Hz, 1H), 6.93 (s, 1H), 6.77 (d, J=7.8 Hz, 1H), 6.65 (dd, J=8.0, 1.6 Hz, 1H), 5.34 (s, 2H). MS (ESI) m/e (M+H+) 260.1.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07659268B2 |
| Source dataset | uspto-grants-2010_02 |
| ORD ID | ord-69053124efc442c6a63df9e0f368191d |
| Source note | uspto-grants-2010_02 |