反应详情

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.

1. temperatureat reflux temperature overnight
2. customAfter the completion of the reaction
3. filtrationfiltered
4. stirringstirred with the saturated aqueous solution of Na2CO3
5. customThe organic layer was separated
6. washwashed with saturated brine
7. dry with materialdried over sodium sulfate
8. concentrationconcentrated