Ethyl Bromide → 2-Bromo-5-ethoxypyridine
反応式
Br[CH2:2][CH3:3].C([O-])([O-])=O.[K+].[K+].[Br:10][C:11]1[CH:16]=[CH:15][C:14]([OH:17])=[CH:13][N:12]=1>C(#N)C>[Br:10][C:11]1[CH:16]=[CH:15][C:14]([O:17][CH2:2][CH3:3])=[CH:13][N:12]=1参加物
5
実験手順
2.51 g (22.99 mmol) 1-bromoethane and 1.99 g (14.37 mmol) K2CO3 are added to a mixture of 1.0 g (5.75 mmol) 2-bromo-5-hydroxypyridine in 100 mL ACN. The mixture is stirred at reflux over night. Then the reaction mixture is poured onto water and extracted with TBME. The organic layer is dried with Na2SO4 and the solvent is removed under vacuo. The residue is purified by column chromatography (silica gel, PE/EtOAC 1/1).
後処理
- temperatureat reflux over night
- additionThen the reaction mixture is poured onto water
- extractionextracted with TBME
- dry with materialThe organic layer is dried with Na2SO4
- customthe solvent is removed under vacuo
- customThe residue is purified by column chromatography (silica gel, PE/EtOAC 1/1)
出典と根拠
- ORDレコード
- ord-36769e8c1de347da8d1796f0a24d3516
- 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…