反应详情

温度

90 °C

To a stirred mixture of 2-iodo-6-methylpyridin-3-ol (530 g, 2.25 mol), Cs2CO3 (876 g, 2.7 mol) and DMF (2.5 L) was added 2-bromo-ethanol (560 g, 4.51 mol) dropwise at 0° C. The mixture was stirred at 90° C. overnight. The reaction was cooled and the solvent was removed in vacuo. The residue was diluted with water (2 L) and the aqueous solution was extracted with CH2Cl2 (3×350 mL). The combined organic layers were washed with brine (2×150 mL), dried over anhydrous Na2SO4 and concentrated to afford 2-(2-iodo-6-methylpyridin-3-yloxy)ethanol (630 g) as a brown solid which was used directly in the next step without further purification.

1. temperatureThe reaction was cooled
2. customthe solvent was removed in vacuo
3. additionThe residue was diluted with water (2 L)
4. extractionthe aqueous solution was extracted with CH2Cl2 (3×350 mL)
5. washThe combined organic layers were washed with brine (2×150 mL)
6. dry with materialdried over anhydrous Na2SO4
7. concentrationconcentrated