HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrogen Bromide → HCID 178503118, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrogen Bromide | HCID 260 | — |
| Reactant | Water | HCID 962 | — |
| Reactant | HCID 21934128 | HCID 21934128 | — |
| Solvent | Acetic Acid | HCID 176 | — |
| Product | HCID 178503118 | HCID 178503118 | 91% |
Reaction Steps
A solution of 2-(2,2,2-Trifluoroethyl)-4-methoxy-5-[4-(methylthio)phenyl]-3(2H)-pyridazinone (2 g, 6.1 mmol) and hydrobromic acid (40% in water, 20 mL) in acetic acid (40 mL) was heated at reflux for 3 hours. The reaction mixture was cooled to room temperature and water (50 mL) was added. The crystals formed were filtered, washed with water and 5% ethyl acetate in hexanes, and dried to constant weight. The product was obtained as a white solid (yield: 1.75 g, 91%). 1H NMR (300 MHz, CDCl3) δ 2.54 (s, 3H), 4.82 (q, J=9 Hz, 2H), 7.47 (d, J=9 Hz, 2H), 7.65 (d, J=9 Hz, 2H), 7.73 (br s, 1H), 8.00 (s, 1H). MS (DCI) m/z 317 (M+H)+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07115591B2 |
| Source dataset | uspto-grants-2006_10 |
| ORD ID | ord-e39bfc21d50c40bab8248f86c58d7d34 |
| Source note | uspto-grants-2006_10 |