Azobisisobutyronitrile → 3-(Bromomethyl)-2-chlorobenzonitrile
反応式
[Cl:1][C:2]1[C:9]([CH3:10])=[CH:8][CH:7]=[CH:6][C:3]=1[C:4]#[N:5].C1C(=O)N([Br:18])C(=O)C1.CC(N=NC(C#N)(C)C)(C#N)C>ClC1C=CC=CC=1>[Br:18][CH2:10][C:9]1[C:2]([Cl:1])=[C:3]([CH:6]=[CH:7][CH:8]=1)[C:4]#[N:5]参加物
5
反応条件
- 温度
- 80 °C
実験手順
A soln. of 2-chloro-3-methylbenzonitrile (6.6 mmol) in 25 mL chlorobenzene was heated to 50° C. when NBS (7.9 mmol) was added. The flask was purged with Ar before AIBN (0.66 mmol) was added at once still at 50° C. The reaction mixture was stirred at 80° C. for 2 h. The solvent was evaporated off, the resulting residue was redissolved in Et2O and washed 3 times with 1N HCl soln. and brine. It was dried over MgSO4 and conc. in vacuo. Purification with CC (0-15% EtOAc/Hept) gives the desired compound as white solid.
後処理
- additionwas added
- additionwas added at once still at 50° C
- customThe solvent was evaporated off
- dissolutionthe resulting residue was redissolved in Et2O
- washwashed 3 times with 1N HCl soln
- dry with materialIt was dried over MgSO4 and conc. in vacuo
- customPurification with CC (0-15% EtOAc/Hept)
出典と根拠
- ORDレコード
- ord-4264d0782815418ba7e31f02a885e5ad
- 出典データセット
- uspto-grants-2016_07
- 特許番号
- US09388197B2
反応ノート
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