Methyl iodide → 5-Chloro-1-methyl-3-nitropyridin-2-one
反応式
[H-].[Na+].[Cl:3][C:4]1[CH:5]=[C:6]([N+:11]([O-:13])=[O:12])[C:7]([OH:10])=[N:8][CH:9]=1.[CH3:14]I>O>[Cl:3][C:4]1[CH:5]=[C:6]([N+:11]([O-:13])=[O:12])[C:7](=[O:10])[N:8]([CH3:14])[CH:9]=1参加物
5
反応条件
- 温度
- 5 °C
実験手順
NaH (52.6 mmol) was slowly added at 5° C. to a solution of 5-chloro-2-hydroxy-3-nitropyridine [21427-61-2] (43.8 mmol) and the mixture was stirred at 5° C. for 30 min. Methyl iodide (65.7 mmol) was added and the mixture was stirred at rt for 20 h. The mixture was diluted with H2O and extracted with EtOAc (3×). The combined organic phases were washed successively with H2O and brine, dried (Na2SO4), filtered and concentrated to afford the title compound. ESI-MS: tR=0.55 min, [M+H]+ 189/191 (LC-MS 1).
後処理
- stirringthe mixture was stirred at rt for 20 h
- extractionextracted with EtOAc (3×)
- washThe combined organic phases were washed successively with H2O and brine
- dry with materialdried (Na2SO4)
- filtrationfiltered
- concentrationconcentrated
出典と根拠
- ORDレコード
- ord-6188df1b48ae4b4a8cc928f679b2d13f
- 出典データセット
- uspto-grants-2016_06
- 特許番号
- US09365576B2
反応ノート
読み込み中…