Isopropyl iodide → Methyl 5-bromo-2-(propan-2-yloxy)pyridine-4-carboxylate
反応式
[Br:1][C:2]1[C:3]([C:9]([O:11][CH3:12])=[O:10])=[CH:4][C:5]([OH:8])=[N:6][CH:7]=1.[CH:13](I)([CH3:15])[CH3:14]>C1(C)C=CC=CC=1>[Br:1][C:2]1[C:3]([C:9]([O:11][CH3:12])=[O:10])=[CH:4][C:5]([O:8][CH:13]([CH3:15])[CH3:14])=[N:6][CH:7]=1参加物
4
実験手順
A solution of methyl 5-bromo-2-hydroxypyridine-4-carboxylate (3.00 g, 12.9 mmol), isopropyl iodide (3.30 g, 19.4 mmol) and Ag2CO3 (4.66 g, 16.8 mmol) in toluene (40 mL) was heated at 100° C. for 2 hours. The solid was filtered through CELITE® and the filtrate was concentrated under vacuum and purified by column chromatography (0-20% ethyl acetate/heptanes) to give methyl 5-bromo-2-(propan-2-yloxy)pyridine-4-carboxylate (112a, 3.5 g, 99%) as a colorless oil.
後処理
- filtrationThe solid was filtered through CELITE®
- concentrationthe filtrate was concentrated under vacuum
- custompurified by column chromatography (0-20% ethyl acetate/heptanes)
出典と根拠
- ORDレコード
- ord-3756b21541054e37bf2286d97908e5b5
- 出典データセット
- uspto-grants-2015_05
- 特許番号
- US09040515B2
反応ノート
読み込み中…