反应详情

温度

0 °C

To a slurry of NaH (1.03 g, 25.8 mmol) in THF (70 mL) was added 1,1,1-trifluoro-2-methylpropan-2-ol (3 g, 23.42 mmol). The reaction was stirred at 0° C. for 20 min. A solution of dipyridin-2-yl carbonate (5.06 g, 23.42 mmol) in THF (30 mL) was then added to the mixture. The resulting solution was stirred at room temperature for overnight. Filtered the resulting solid byproducts and washed with EtOAc (2×20 mL). The combined organic layers was washed with water, dried over anhydrous Na2SO4, filtered and concentrated under reduced pressure. The resulting white pyridin-2-yl (1,1,1-trifluoro-2-methylpropan-2-yl) carbonate (1.24 g, 21%) was directly used as a reagent.

1. stirringThe resulting solution was stirred at room temperature for overnight
2. filtrationFiltered the resulting solid byproducts
3. washwashed with EtOAc (2×20 mL)
4. washThe combined organic layers was washed with water
5. dry with materialdried over anhydrous Na2SO4
6. filtrationfiltered
7. concentrationconcentrated under reduced pressure