HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → 2-(2,2,2-Trifluoroethyl)-2-(trifluoromethyl)-1,3-benzodioxole
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | 2-(1-Chloro-2,2,2-trifluoroethyl)-2-trifluoromethyl-1,3-benzodioxole | HCID 54455048 | — |
| Reactant | HCID 178418361 | HCID 178418361 | — |
| Catalyst | Palladium | HCID 23938 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | 2-(2,2,2-Trifluoroethyl)-2-(trifluoromethyl)-1,3-benzodioxole | HCID 53667303 | — |
Reaction Steps
306.5 g of 2-(1-chloro-2,2,2-trifluoroethyl)-2-trifluoromethyl-1,3-benzodioxole from Example 2a were dissolved in 500 ml of THF, and 101 g of triethylamine and 30 g of palladium on carbon (5% by weight) were added. Hydrogenation was then carried out with 100 bar of hydrogen at 110° C. for 48 h. The mixture was then filtered, the solvent stripped off in vacuo and the residue subjected to fractional distillation in vacuo. The yield was 126 g (46% of theory) and the boiling point was 60° C. at 10 mbar. The NMR spectra showed the following characteristic absorption: 19F-NMR: -59.0 and -84.6 ppm; 1H-NMR: 3.02 ppm.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05877195 |
| Source dataset | uspto-grants-1999_03 |
| ORD ID | ord-34954e7e5e1f432fbf0687756a7a254a |
| Source note | uspto-grants-1999_03 |