HuagongsheHuagongshe Chemistry Print Report · For research reference only
Acetic Acid → HCID 68305187, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Acetic Acid | HCID 176 | — |
| Reactant | [(2E)-3-(dimethylamino)-2-(trifluoromethyl)prop-2-en-1-ylidene]dimethylazanium; hexafluoro-lambda5-phosphanuide | HCID 15877725 | — |
| Reactant | HCID 178509245 | HCID 178509245 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | HCID 68305187 | HCID 68305187 | 88.3% |
Reaction Steps
3-Amino-4-bromopyrazole (4.29, 26.5 mmol) and 2-(trifluoromethyl)-1,3-bis(dimethylamino)trimethinium hexafluorophosphate (9.00 g, 26.5 mmol) were dissolved in ethanol (52.9 mL) and acetic acid (35.3 mL) and the reaction heated to 70° C. for 16 h. The solution was cooled to room temperature and concentrated. The residue was filtered through a fritted funnel, the precipitate washed with water, and dried under reduced pressure to afford the title compound (6.22 g, 23.4 mmol). LRMS (APCI) calc'd for (C7H3BrF3N3) [M+H]+, 266.0; found 265.9. 1H NMR (CDCl3, 500 MHz) δ 8.96 (d, J=1.1, 2.1, 1H), 8.71 (d, J=2.1, 1H), 8.28 (s, 1H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08946237B2 |
| Source dataset | uspto-grants-2015_02 |
| ORD ID | ord-b76cec3d45704f3d82822b5103fdff59 |
| Source note | uspto-grants-2015_02 |