2-Bromo-4-methylaniline → 2-Amino-5-methylbenzonitrile
反応式
Br[C:2]1[CH:7]=[C:6]([CH3:8])[CH:5]=[CH:4][C:3]=1[NH2:9].[C:10]([Cu])#[N:11]>CN1C(=O)CCC1>[NH2:9][C:3]1[CH:4]=[CH:5][C:6]([CH3:8])=[CH:7][C:2]=1[C:10]#[N:11]参加物
4
実験手順
Combine 2-bromo-4-methyl-phenylamine (8.00 g, 43.0 mmol), CuCN (4.62 g, 51.6 mmol), and NMP (30.0 ml) and stir at reflux. After 75 minutes, cool to ambient temperature, pour the mixture onto ice chips and stir for 1 hour. Remove the resulting precipitate by vacuum filtration. Dissolve the precipitate in NH4OH and extract with dichloromethane. Combine, wash (brine), dry (sodium sulfate), and reduce the extracts to residue. Purify the residue on silica gel using dichloromethane/hexanes (75:25) to give 3.39 g (60%) of an orange solid: mass spectrum (ion spray): m/z=133.1 (M+1).
後処理
- temperatureat reflux
- additionpour the mixture onto ice chips
- customRemove the resulting precipitate
- filtrationby vacuum filtration
- dissolutionDissolve the precipitate in NH4OH
- extractionextract with dichloromethane
- washCombine, wash (brine)
- dry with materialdry (sodium sulfate)
- customPurify the residue on silica gel
出典と根拠
- ORDレコード
- ord-04bb8768009749168397a3561c82c357
- 出典データセット
- uspto-grants-2008_06
- 特許番号
- US07384934B2
反応ノート
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