2-Methoxyethanol → 5-Bromo-2-(2-methoxyethoxy)pyridine
反応式
[CH3:1][O:2][CH2:3][CH2:4][OH:5].[H-].[Na+].C1COCC1.Br[C:14]1[CH:19]=[CH:18][C:17]([Br:20])=[CH:16][N:15]=1>C([O-])(O)=O.[Na+]>[Br:20][C:17]1[CH:18]=[CH:19][C:14]([O:5][CH2:4][CH2:3][O:2][CH3:1])=[N:15][CH:16]=1参加物
6
実験手順
0.25 mL 2-methoxyethanol (3.17 mmol) are added to a mixture of 80 mg (3.17 mmol) sodium hydride and 5 mL THF. The mixture is stirred at rt for 10 min. Subsequently, 500 mg (2.11 mmol) 2,5-dibromopyridine are added and the mixture is stirred for 5 h at 75° C. After that time, the reaction mixture is diluted with sat. aq. NaHCO3 solution and extracted with EtOAc. The organic layer is dried over magnesium sulphate and the solvent is removed in vacuo. The crude product is purified by column chromatography (silica gel, PE/EtOAc 85/15).
後処理
- stirringthe mixture is stirred for 5 h at 75° C
- extractionextracted with EtOAc
- dry with materialThe organic layer is dried over magnesium sulphate
- customthe solvent is removed in vacuo
- customThe crude product is purified by column chromatography (silica gel, PE/EtOAc 85/15)
出典と根拠
- ORDレコード
- ord-fef4f21f5ac54b9189cbdb31ce4a5c00
- 出典データセット
- uspto-grants-2014_11
- 特許番号
- US08877754B2
反応ノート
読み込み中…