HuagongsheHuagongshe Chemistry Print Report · For research reference only
4-Chloro-3-(trifluoromethyl)benzyl alcohol → 4-(Hydroxymethyl)-2-(trifluoromethyl)benzonitrile
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 4-Chloro-3-(trifluoromethyl)benzyl alcohol | HCID 2778111 | — |
| Reactant | HCID 178514179 | HCID 178514179 | — |
| Catalyst | Tetrakis(triphenylphosphine)palladium | HCID 11979704 | — |
| Solvent | Dimethylacetamide | HCID 31374 | — |
| Product | 4-(Hydroxymethyl)-2-(trifluoromethyl)benzonitrile | HCID 67211929 | 36.6% |
Reaction Conditions
| Temperature | 150 °C |
|---|
Reaction Steps
To a solution of (4-chloro-3-(trifluoromethyl)phenyl)methanol (0.300 g, 1.425 mmol) in DMA was added dicyanozinc (0.335 g, 2.85 mmol) and tetrakis(triphenylphosphine) palladium (0) (0.165 g, 0.142 mmol). The reaction flask was degassed and charged with nitrogen, then heated at 150° C. for 6 h under microwave irradiation. The reaction mixture was poured into water and extracted with EtOAc. The EtOAc extract was washed with brine, dried over MgSO4 and purified by silica gel column chromatography to give the title compound as a white solid (0.105 g). LCMS m/z=202.1 [M+H]+. 1H NMR (400 MHz, CDCl3) δ ppm 1.98 (bs, 1H), 4.87 (s, 2H), 7.69 (d, J=0.88 Hz, 1H), 7.77-7.88 (m, 2H)
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09126932B2 |
| Source dataset | uspto-grants-2015_09 |
| ORD ID | ord-c72addd12d1f452fa88a37838e4d033c |
| Source note | uspto-grants-2015_09 |