Triethylamine → 3-Bromo-6-chloro-4-methylpyridine-2-carbonitrile
反応式
[Br:1][C:2]1[C:3]([CH3:10])=[CH:4][C:5]([Cl:9])=[N+:6]([O-])[CH:7]=1.[Si]([C:15]#[N:16])(C)(C)C.C(N(CC)CC)C>C(#N)C>[Br:1][C:2]1[C:7]([C:15]#[N:16])=[N:6][C:5]([Cl:9])=[CH:4][C:3]=1[CH3:10]参加物
5
反応条件
- 温度
- 100 °C
実験手順
To a solution of 5-bromo-2-chloro-4-methylpyridine 1-oxide (from step 1) (1.0 eq.) in acetonitrile (0.2 M) was added TMSCN (4.0 eq.) and triethylamine (3.0 eq.). The reaction was heated at 100° C. overnight. After cooling to room temperature, the solvent was concentrated en vacuo, and the residue was purified by a COMBIFLASH® system (ISCO) using 0-50% ethyl acetate in hexane to give 3-bromo-6-chloro-4-methylpicolinonitrile.
後処理
- temperatureAfter cooling to room temperature
- concentrationthe solvent was concentrated en vacuo
- customthe residue was purified by a COMBIFLASH® system (ISCO)
出典と根拠
- ORDレコード
- ord-f51ec58fbb9540f1b9c383f14a4cb579
- 出典データセット
- uspto-grants-2014_11
- 特許番号
- US08895577B2
反応ノート
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