2-Methoxyethanol → 5-Bromo-2-(2-methoxyethoxy)pyridine
反応式
[CH3:1][O:2][CH2:3][CH2:4][OH:5].[H-].[Na+].Br[C:9]1[CH:14]=[CH:13][C:12]([Br:15])=[CH:11][N:10]=1>C1COCC1>[Br:15][C:12]1[CH:13]=[CH:14][C:9]([O:5][CH2:4][CH2:3][O:2][CH3:1])=[N:10][CH:11]=1参加物
5
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 in 5 mL THF. The reaction mixture is stirred at r.t. for 10 min before 500 mg (2.11 mmol) 2,5-dibromopyridine are added. After 5 h at 75° C. the reaction mixture is diluted with half sat.aq. NaHCO3 solution and extracted with EtOAc. The organic layer is dried with MgSO4 and the solvent is removed in vacuo. The crude product is purified by column chromatography (silica gel, PE/EtOAc 85/15).
後処理
- additionare added
- additionAfter 5 h at 75° C. the reaction mixture is diluted with half sat.aq
- extractionNaHCO3 solution and extracted with EtOAc
- dry with materialThe organic layer is dried with MgSO4
- 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-c63a91032d1f4a6fa94b0f90a8a2f920
- 出典データセット
- uspto-grants-2014_09
- 特許番号
- US08835472B2
反応ノート
読み込み中…