HuagongsheHuagongshe Chemistry Print Report · For research reference only
5-Nitro-2-(2,2,2-trifluoroethyl)-2-trifluoromethyl-1,3-benzodioxole → 5-Amino-2-(2,2,2-trifluoroethyl)-2-trifluoromethyl-1,3-benzodioxole
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 5-Nitro-2-(2,2,2-trifluoroethyl)-2-trifluoromethyl-1,3-benzodioxole | HCID 53877230 | — |
| Reactant | HCID 178418361 | HCID 178418361 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | 5-Amino-2-(2,2,2-trifluoroethyl)-2-trifluoromethyl-1,3-benzodioxole | HCID 54171543 | 71.2% |
Reaction Steps
57.4 g of the product from Example 15a were dissolved in 400 ml of tetrahydrofuran and hydrogenated in the presence of 4 g of catalyst (palladium on carbon, 10% by weight) for 5 hours at 30° C. at 50 bar with hydrogen. The mixture was then filtered, the solvent removed, and the remaining filtrate distilled under a high vacuum. 37 g of product (=63% of theory) were obtained with a boiling point of 83° C. at 0.07 mbar. 19F-NMR: -59.0 and -84.6 ppm; 1H-NMR: 2.98 ppm.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05585395 |
| Source dataset | uspto-grants-1996_12 |
| ORD ID | ord-1ba835f74877438b9fdc4916160febb3 |
| Source note | uspto-grants-1996_12 |