Ammonium Chloride → 1-(2,6-Dichloropyridin-4-YL)ethanone
反応式
[Cl:1][C:2]1[CH:3]=[C:4]([CH:11]=[C:12]([Cl:14])[N:13]=1)[C:5](N(OC)C)=[O:6].O1CCC[CH2:16]1.C[Mg]Br.[Cl-].[NH4+]>O1CCCC1.C(OCC)(=O)C>[Cl:1][C:2]1[CH:3]=[C:4]([C:5](=[O:6])[CH3:16])[CH:11]=[C:12]([Cl:14])[N:13]=1参加物
6
反応条件
- 温度
- 0 °C
実験手順
490 mg of 2,6-dichloro-N-methoxy-N-methyl isonicotinamide was dissolved in tetrahydrofuran, 2.1 ml of 3M methyl magnesium bromide tetrahydrofuran solution was added dropwise at 0° C., and the mixture was stirred at 0° C. for 1 hour. To the reaction solution was added ammonium chloride aqueous solution, and the mixture was diluted with ethyl acetate. The mixture was washed with brine, and then dried over magnesium sulfate. The solvent was distilled off under reduced pressure to obtain 325 mg of the objective compound.
後処理
- washThe mixture was washed with brine
- dry with materialdried over magnesium sulfate
- distillationThe solvent was distilled off under reduced pressure
出典と根拠
- ORDレコード
- ord-4ba0665576fc45e789e091e37966bd77
- 出典データセット
- uspto-grants-2014_03
- 特許番号
- US08673891B2
反応ノート
読み込み中…