Hydrogen Bromide → 6-Bromo-8-iodoimidazo[1,2-a]pyridine
反応式
[Br:1][C:2]1[CH:3]=[C:4]([I:9])[C:5]([NH2:8])=[N:6][CH:7]=1.Br[CH2:11][CH:12](OC)OC.Br>C(O)C.O>[Br:1][C:2]1[CH:3]=[C:4]([I:9])[C:5]2[N:6]([CH:11]=[CH:12][N:8]=2)[CH:7]=1参加物
6
実験手順
5-bromo-3-iodopyridin-2-amine (1.0 g, 3.34 mmol) and 2-bromo-1,1-dimethoxyethane were dissolved in ethanol (20 ml). To this solution was added a 50% mixture of HBr in water (4 ml). The mixture was stirred at reflux temperature overnight. After the completion of the reaction, the mixture was cooled to room temperature and filtered. The residue was suspended in DCM (10 ml) and stirred with the saturated aqueous solution of Na2CO3. The organic layer was separated and washed with saturated brine, dried over sodium sulfate and concentrated. The desired product was obtained as a yellow solid (950 mg, yield 88%). LC-MS: 323 [M+1]+, tR=1.299 min.
後処理
- temperatureat reflux temperature overnight
- customAfter the completion of the reaction
- filtrationfiltered
- stirringstirred with the saturated aqueous solution of Na2CO3
- customThe organic layer was separated
- washwashed with saturated brine
- dry with materialdried over sodium sulfate
- concentrationconcentrated
出典と根拠
- ORDレコード
- ord-86e5b1beb5d540a2900b38aa5704dcc6
- 出典データセット
- uspto-grants-2014_06
- 特許番号
- US08742098B2
反応ノート
読み込み中…