Dimethylcarbamoyl Chloride → 4,5-Dimethylpyridine-2-carbonitrile
反応式
[CH3:1][C:2]1[CH:3]=[N+:4]([O-])[CH:5]=[CH:6][C:7]=1[CH3:8].[CH3:10][N:11](C)C(Cl)=O.C[Si](C#N)(C)C>C(Cl)Cl>[C:10]([C:5]1[N:4]=[CH:3][C:2]([CH3:1])=[C:7]([CH3:8])[CH:6]=1)#[N:11]参加物
5
実験手順
17.8 g of the obtained 3,4-dimethylpyridine-N-oxide (144.5 mmol) was dissolved under an argon gas atmosphere in 250 mL of methylene dichloride, added thereto 13.2 mL of dimethyl carbamoyl chloride (144 mmol), then 19.0 mL of trimethylsilyl cyanide (152 mmol), and stirred overnight at room temperature. The reaction solution was quenched with 10%-K2CO3 aqueous solution, the methylene dichloride layer was separated, dried on salt cake and concentrated to give 3.40 g of 6-cyano-3,4-dimethylpyridine (18% yield).
後処理
- additionadded
- customThe reaction solution was quenched with 10%-K2CO3 aqueous solution
- customthe methylene dichloride layer was separated
- customdried on salt cake
- concentrationconcentrated
出典と根拠
- ORDレコード
- ord-c7130fc8c111404c873fc7fd6081327f
- 出典データセット
- uspto-grants-2015_11
- 特許番号
- US09174906B2
反応ノート
読み込み中…