N-bromobutanimide → 3-Bromo-7-thiazol-2-yl-imidazo[1,2-a]pyridine
反応式
[S:1]1[CH:5]=[CH:4][N:3]=[C:2]1[C:6]1[CH:11]=[CH:10][N:9]2[CH:12]=[CH:13][N:14]=[C:8]2[CH:7]=1.C1C(=O)N([Br:22])C(=O)C1>C(O)C.ClCCl>[Br:22][C:12]1[N:9]2[CH:10]=[CH:11][C:6]([C:2]3[S:1][CH:5]=[CH:4][N:3]=3)=[CH:7][C:8]2=[N:14][CH:13]=1参加物
5
実験手順
Dissolve 7-thiazol-2-yl-imidazo[1,2-a]pyridine (1.14 g, 5.66 mmol) in 25 mL absolute ethanol, then add NBS (1.0 g, 5.66 mmol), stir the mixture at room temperature for 15 minutes, dilute with 35 mL dichloromethane and apply to a 10 g SCX Mega Bond-Elut™ cartridge (Varian) pre-washed with 150 mL 1:1 CH2Cl2:MeOH. Wash the SCX cartridge with 300 mL 1:1 CH2Cl2:MeOH, elute with 150 mL CH2Cl2:2 M NH3-MeOH, and concentrate the eluates and dry to provide 1.07 g (67%) of the title compound as a tan solid. MS (ES) 280, 282.
後処理
- washpre-washed with 150 mL 1:1 CH2Cl2
- washWash the SCX cartridge with 300 mL 1:1 CH2Cl2
- washMeOH, elute with 150 mL CH2Cl2
- concentration2 M NH3-MeOH, and concentrate the eluates
- customdry
出典と根拠
- ORDレコード
- ord-21a2d8e681ab4c06a3299f810d10953b
- 出典データセット
- uspto-grants-2010_02
- 特許番号
- US07666879B2
反応ノート
読み込み中…