Methyl iodide → (5-Bromo-6-hydroxy-pyridin-3-yl)-acetic acid ethyl ester
反応式
[CH2:1]([O:3][C:4](=[O:15])[CH2:5][C:6]1[CH:7]=[N:8][C:9]([O:13]C)=[C:10]([Br:12])[CH:11]=1)[CH3:2].IC>C(Cl)(Cl)Cl.C(=O)([O-])[O-].[Ag+2]>[CH2:1]([O:3][C:4](=[O:15])[CH2:5][C:6]1[CH:7]=[N:8][C:9]([OH:13])=[C:10]([Br:12])[CH:11]=1)[CH3:2]参加物
5
反応条件
- 温度
- 55 °C
実験手順
(5-Bromo-6-methoxy-pyridin-3-yl)-acetic acid ethyl ester (5.02 mmol) was dissolved in CHCl3 (17 mL). Silver carbonate (1.58 g, 5.7 mmol) and iodomethane (0.82 mL, 13.14 mmol) were added, and the reaction was stirred at 55° C. for 2.5 hours. The mixture was filtered through Celite, and the filtrate was concentrated and purified by silica gel chromatography (0-60% EtOAc in hexanes) to give (5-bromo-6-hydroxy-pyridin-3-yl)-acetic acid ethyl ester.
後処理
- filtrationThe mixture was filtered through Celite
- concentrationthe filtrate was concentrated
- custompurified by silica gel chromatography (0-60% EtOAc in hexanes)
出典と根拠
- ORDレコード
- ord-7448f2e808114f2abd30cf986c23124b
- 出典データセット
- uspto-grants-2011_11
- 特許番号
- US08049015B2
反応ノート
読み込み中…