N-bromobutanimide → 3-Bromo-7-chloroimidazo[1,2-a]pyridine
反応式
[Cl:1][C:2]1[CH:7]=[CH:6][N:5]2[CH:8]=[CH:9][N:10]=[C:4]2[CH:3]=1.C1C(=O)N([Br:18])C(=O)C1>CN(C=O)C.CCOC(C)=O>[Br:18][C:8]1[N:5]2[CH:6]=[CH:7][C:2]([Cl:1])=[CH:3][C:4]2=[N:10][CH:9]=1参加物
5
反応条件
- 温度
- 0 °C
実験手順
7-Chloro-imidazo-[1,2-a]-pyridine (1 eq, 38.9 mmol, 5.93 g) is dissolved in DMF (20 ml) at 0° C. and NBS (1.1 eq, 42.8 mmol, 7.61 g) is added. The reaction mixture is stirred for 1 h at 0° C. and is diluted with EtOAc. The reaction mixture is washed with NaHCO3 and brine, dried over MgSO4, filtered and evaporated. The product is purified by flash column chromatography eluting with 8:2 DCM/MeOH to afford 3-bromo-7-chloro-imidazo-[1,2-a]-pyridine as a brown solid; [M+H]+=232
後処理
- washThe reaction mixture is washed with NaHCO3 and brine
- dry with materialdried over MgSO4
- filtrationfiltered
- customevaporated
- customThe product is purified by flash column chromatography
- washeluting with 8:2 DCM/MeOH
出典と根拠
- ORDレコード
- ord-01a95fab00f84eef93eab8aa5a019c69
- 出典データセット
- uspto-grants-2013_02
- 特許番号
- US08367662B2
反応ノート
読み込み中…