Methyl iodide → 5-Bromo-1,6-dimethyl-1H-pyridin-2-one
反応式
[Br:1][C:2]1[CH:3]=[CH:4][C:5](=[O:9])[NH:6][C:7]=1[CH3:8].IC.[C:12]([O-])([O-])=O.[K+].[K+]>CS(C)=O>[Br:1][C:2]1[CH:3]=[CH:4][C:5](=[O:9])[N:6]([CH3:12])[C:7]=1[CH3:8]参加物
5
反応条件
- 温度
- 60 °C
実験手順
To a solution of 5-bromo-6-methylpyridin-2(1H)-one (164 mg, 0.872 mmol) and iodomethane (0.065 mL, 1.047 mmol) in DMSO (3 mL) was added K2CO3 (145 mg, 1.047 mmol). The mixture was stirred at 60° C. overnight, filtered, and purified via preparative HPLC, eluting with a gradient of 20-70% ACN (containing 0.035% TFA) in H2O (containing 0.05% TFA) to give the title compound.
後処理
- filtrationfiltered
- custompurified via preparative HPLC
- washeluting with a gradient of 20-70% ACN (containing 0.035% TFA) in H2O (containing 0.05% TFA)
出典と根拠
- ORDレコード
- ord-dd0bac2e0d6f483b8c081e4f44f0112d
- 出典データセット
- uspto-grants-2016_09
- 特許番号
- US09434743B2
反応ノート
読み込み中…