Azobisisobutyronitrile → 1-(Bromomethyl)-2-iodo-3-nitro-5-(trifluoromethyl)benzene
反応式
[CH3:1][C:2]1[CH:7]=[C:6]([C:8]([F:11])([F:10])[F:9])[CH:5]=[C:4]([N+:12]([O-:14])=[O:13])[C:3]=1[I:15].C1C(=O)N([Br:23])C(=O)C1.CC(N=NC(C#N)(C)C)(C#N)C>C(Cl)(Cl)(Cl)Cl>[Br:23][CH2:1][C:2]1[CH:7]=[C:6]([C:8]([F:11])([F:9])[F:10])[CH:5]=[C:4]([N+:12]([O-:14])=[O:13])[C:3]=1[I:15]参加物
5
実験手順
A mixture of the title compound from Step C (0.38 g, 1.15 mmol), NBS (0.24 g, 1.38 mmol) and catalytic amount of AIBN in carbon tetrachloride (5 ml) was heated to reflux for 3 days. During the period more AIBN was added daily. The mixture was cooled and concentrated. The title compound was obtained after flash column using hexane as the eluant. 1H NMR (CDCl3, 500 MHz): δ 7.91 (s, 1H), 7.80 (s, 1H), 4.75 (s, 2H).
後処理
- temperaturewas heated
- temperatureto reflux for 3 days
- temperatureThe mixture was cooled
- concentrationconcentrated
出典と根拠
- ORDレコード
- ord-025265677ad142828cfccc0eb2228fdd
- 出典データセット
- uspto-grants-2013_05
- 特許番号
- US08440702B2
反応ノート
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