HuagongsheHuagongshe Chemistry Print Report · For research reference only
Azobisisobutyronitrile → (6-Bromo-3-bromomethyl-benzofuran-2-yl)(2,4-dichlorophenyl)-methanone
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Azobisisobutyronitrile | HCID 6547 | — |
| Reactant | N-bromobutanimide | HCID 67184 | — |
| Reactant | (6-Bromo-3-methyl-benzofuran-2-yl)(2,4-dichloro-phenyl)methanone | HCID 59788907 | — |
| Solvent | Carbon Tetrachloride | HCID 5943 | — |
| Product | (6-Bromo-3-bromomethyl-benzofuran-2-yl)(2,4-dichlorophenyl)-methanone | HCID 59788888 | 68.5% |
Reaction Steps
To a stirred solution of (6-Bromo-3-methyl-benzofuran-2-yl)-(2,4-dichloro-phenyl)-methanone (4.0 g, 10.4 mmol) in carbon tetrachloride (40 mL) was added 2,2′-azobisisobutyronitrile (AIBN) (171 mg, 1.04 mmol) and N-bromosuccinimide (1.95 g, 10.9 mmol). The reaction mixture was heated at reflux for 6 h, and upon cooling to rt, the resulting precipitate was removed by filtration and the filtrate was concentrated. The crude residue was purified by column chromatography (10% ethyl acetate in hexanes) to afford the desired product (3.30 g, 65% yield) as a white solid. Rf=0.68 (10% EtOAc in hexanes). 1H-NMR (acetone): δ 7.98(d, 1H), 7.91 (s, 1H), 7.74 (m, 2H), 7.64 (td, 2H), 5.16 (s, 2H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07420066B2 |
| Source dataset | uspto-grants-2008_09 |
| ORD ID | ord-20639e06089d4185a6519fa1fc357550 |
| Source note | uspto-grants-2008_09 |