2-Pyridinamine, 5-iodo- → Ethyl 6-iodoimidazo[1,2-a]pyridine-3-carboxylate
反応式
[CH2:1]([O:3][C:4](=[O:8])[CH2:5][CH:6]=O)[CH3:2].[NH2:9][C:10]1[CH:15]=[CH:14][C:13]([I:16])=[CH:12][N:11]=1.C(#N)C.C(O)C>C(=O)(O)[O-].[Na+]>[CH2:1]([O:3][C:4]([C:5]1[N:11]2[CH:12]=[C:13]([I:16])[CH:14]=[CH:15][C:10]2=[N:9][CH:6]=1)=[O:8])[CH3:2]参加物
5
実験手順
Reflux a solution of 3-oxo-propionic acid ethyl ester (J. Med. Chem. 2001, 44(12), 1193-2003; 3.4 g, 23.7 mmol) and 2-amino-5-iodopyridine in 1:1 acetonitrile/ethanol (100 mL) overnight. Dilute with saturated aqueous sodium bicarbonate, extract into dichloromethane (4×100 mL), combine organics, and concentrate. Flash chromatography using appropriate ethyl acetate/hexane mixtures gives 3.7 g (78%) of the subtitled compound as an off-white solid. ES+ m/e 316.7 (M+1).
後処理
- extractionextract into dichloromethane (4×100 mL)
- concentrationconcentrate
出典と根拠
- ORDレコード
- ord-4143c9f7f2824ec8934c2853a1f0931c
- 出典データセット
- uspto-grants-2008_07
- 特許番号
- US07405299B2
反応ノート
読み込み中…