HuagongsheHuagongshe Chemistry Print Report · For research reference only
Nitric Acid → 5,6-Dinitro-2-(2,2,2-trifluoroethyl)-2-(trifluoromethyl)-1,3-benzodioxole
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Nitric Acid | HCID 944 | — |
| Reactant | 5-Nitro-2-(2,2,2-trifluoroethyl)-2-trifluoromethyl-1,3-benzodioxole | HCID 53877230 | — |
| Solvent | Sulfuric Acid | HCID 1118 | — |
| Product | 5,6-Dinitro-2-(2,2,2-trifluoroethyl)-2-(trifluoromethyl)-1,3-benzodioxole | HCID 53660706 | — |
Reaction Steps
A mixture of 250 ml of 100% strength by weight nitric acid and 350 ml of concentrated sulphuric acid was added dropwise with stirring to an initial charge of 317 g of the product from Example 15a. The mixture was stirred for 2 hours at 55° C. The mixture was then cooled and poured into ice-water. The product was extracted with methylene chloride, washed until neutral with sodium hydrogen carbonate solution, dried, and freed on a rotary evaporator from readily volatile constituents. The yield was 339 g (=94% of theory), the melting point was 101° to 103° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05585395 |
| Source dataset | uspto-grants-1996_12 |
| ORD ID | ord-0e60ad0849ee405a87c86c2dd4a42022 |
| Source note | uspto-grants-1996_12 |