Azobisisobutyronitrile → Methyl 2-(bromomethyl)-6-cyanobenzoate
反応式
[C:1]([C:3]1[CH:12]=[CH:11][CH:10]=[C:9]([CH3:13])[C:4]=1[C:5]([O:7][CH3:8])=[O:6])#[N:2].[Br:14]N1C(=O)CCC1=O.CC(N=NC(C#N)(C)C)(C#N)C>C(Cl)(Cl)Cl>[Br:14][CH2:13][C:9]1[CH:10]=[CH:11][CH:12]=[C:3]([C:1]#[N:2])[C:4]=1[C:5]([O:7][CH3:8])=[O:6]参加物
5
実験手順
To a solution of EXAMPLE 6B (2.37 g) in chloroform (30 mL) was added N-bromosuccinimide (2.41 g) and AIBN (4 mg), and the mixture was heated at reflux for 18 hours. After cooling, the solvent was removed, and the concentrate was partitioned between ethyl acetate and water. The extract was washed with brine and concentrated, and the concentrate was purified by flash chromatography on silica gel with 20% ethyl acetate in hexanes.
後処理
- temperaturethe mixture was heated
- temperatureat reflux for 18 hours
- temperatureAfter cooling
- customthe solvent was removed
- customthe concentrate was partitioned between ethyl acetate and water
- washThe extract was washed with brine
- concentrationconcentrated
- customthe concentrate was purified by flash chromatography on silica gel with 20% ethyl acetate in hexanes
出典と根拠
- ORDレコード
- ord-8fe6d4d1f682457f9724a30085ca1786
- 出典データセット
- uspto-grants-2012_03
- 特許番号
- US08143284B2
反応ノート
読み込み中…