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>CN(C=O)C>[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
A mixture of NaH (577 mg, 14.4 mmol) and 5-chloro-2-hydroxy-3-nitropyridine (2.1 g, 12.0 mmol) in DMF (21 mL) was stirred for 1 h at 5° C. Methyl iodide (1.1 mL, 18.0 mmol) was added. The resulting mixture was allowed to warm to rt, stirred overnight, cooled to 0° C., quenched by addition of water, and extracted with EtOAc. The organic layer was dried (Na2SO4), filtered, and concentrated. The residue was used without further purification. tR: 0.61 min (LC-MS 2); ESI-MS: 189.1/191.1 [M+H]+ (LC-MS 2).
後処理
- temperatureto warm to rt
- stirringstirred overnight
- temperaturecooled to 0° C.
- customquenched by addition of water
- extractionextracted with EtOAc
- dry with materialThe organic layer was dried (Na2SO4)
- filtrationfiltered
- concentrationconcentrated
- customThe residue was used without further purification
出典と根拠
- ORDレコード
- ord-de86455240f14e0db4e69d55d7d77106
- 出典データセット
- uspto-grants-2014_08
- 特許番号
- US08815926B2
反応ノート
読み込み中…