HuagongsheHuagongshe Chemistry Print Report · For research reference only
p-Bromoacetophenone → 1-[4-(1H-1,2,4-Triazol-1-yl)phenyl]ethan-1-one
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | p-Bromoacetophenone | HCID 7466 | — |
| Reactant | 1H-1,2,4-Triazole | HCID 9257 | — |
| Reactant | Cesium carbonate | HCID 10796 | — |
| Catalyst | Copper(1+) iodide; Copper(I) iodide; Cuprous iodide; Cuprous iodide (CuI) | HCID 24350 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | 1-[4-(1H-1,2,4-Triazol-1-yl)phenyl]ethan-1-one | HCID 2560317 | 96% |
Reaction Steps
To a stirred solution of 4-bromoacetophenone (10 g, 50 mmol) in DMF (100 mL), were added 1,2,4-triazole (5 g, 75 mmol), Cs2CO3 (32.6 g, 100.5 mmol) and CuI (1.4 g, 10.1 mmol) and the resultant reaction mixture was refluxed for 48 h. After completion of the reaction (by TLC), the reaction mixture was cooled to ambient temperature and diluted with water (200 mL) and extracted with EtOAc. The combined organic layer was washed with brine and dried over Na2SO4 and concentrated under reduced pressure. Purification by washing with Et2O afforded the title compound as a solid (5 g, 96%): 1H NMR (400 MHz, CDCl3) δ 8.71 (s, 1H), 8.16, (s, 1H), 8.13 (d, J=8.6 Hz, 2H), 7.83 (d, J=8.6 Hz, 2H), 2.66 (s, 3H); ESIMS m/z 186.02 ([M−H]−).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09226500B2 |
| Source dataset | uspto-grants-2016_01 |
| ORD ID | ord-a5cbdb5ac4bf45138060666595c3aac6 |
| Source note | uspto-grants-2016_01 |