反应详情

To a 1 liter round bottom flask fitted with a condenser, nitrogen inlet, and magnetic stir bar is added 4-[2-(2,4-Difluoro-phenyl)-1-methoxycarbonyl-2-oxo-ethylcarbamoyl]-piperidine-1-carboxylic acid benzyl ester, (32 g, 67.4 mmol), and 120 mL of thionyl chloride. The mixture is immersed in an oil bath preheated to 70° C. and stirred for 10 minutes. The reaction is removed, cooled to room temperature and concentrated to an amber oil. The amber oil is carefully treated with about 50 g of ice, and 350 mL of saturated sodium bicarbonate. The resulting mixture is extracted with 3×100 mL of diethyl ether. The organic layers are combined, washed with brine, dried over magnesium sulfate and concentrated to a thick amber paste to yield the title compound.

1. customTo a 1 liter round bottom flask fitted with a condenser, nitrogen inlet, and magnetic stir bar
2. customThe mixture is immersed in an oil bath
3. custompreheated to 70° C.
4. customThe reaction is removed
5. concentrationconcentrated to an amber oil
6. additionThe amber oil is carefully treated with about 50 g of ice, and 350 mL of saturated sodium bicarbonate
7. extractionThe resulting mixture is extracted with 3×100 mL of diethyl ether
8. washwashed with brine
9. dry with materialdried over magnesium sulfate
10. concentrationconcentrated to a thick amber paste