反应详情

温度

50 °C

To a solution of (2-bromo-3-pyridyl)methyl methanesulfonate (2.5 g, 9.39 mmol) in ethanol (46.97 mL) at room temperature, potassium carbonate (2.62 g) and 1H-imidazole (1.31 g) are added. The mixture is stirred at 50° C. A thick sort of emulsion is formed and 10 mL of ethanol is added and the kind of emulsion is stirred at 50° C. overnight. Water is added until all solids are dissolved. Then, it is concentrated under reduced pressure and the residue is diluted with ethyl acetate and washed with sodium bicarbonate (saturated aqueous solution). Organic layer is decanted, dried over magnesium sulfate and solvent evaporated in vacuo. Crude material is purified by normal phase Isco chromatography using as eluent dichloromethane and methanol (98/2 to 90/10) to yield 1.42 g of the title compound. MS (m/z): 238, 240 (M+1, M+3).

1. customA thick sort of emulsion is formed
2. stirringthe kind of emulsion is stirred at 50° C. overnight
3. dissolutionare dissolved
4. concentrationThen, it is concentrated under reduced pressure
5. additionthe residue is diluted with ethyl acetate
6. washwashed with sodium bicarbonate (saturated aqueous solution)
7. customOrganic layer is decanted
8. dry with materialdried over magnesium sulfate and solvent
9. customevaporated in vacuo
10. customCrude material is purified by normal phase Isco chromatography