反应详情

温度

0 °C

55 ml (0.11 mmol) of 2 M lithium diisopropylamide are added with stirring at −70° C. to a solution of 19.3 g (0.1 mmol) of 1-bromo-3,5-difluorobenzene in 120 ml of dried tetrahydrofuran. After 30 minutes, N-formylpiperidine is added dropwise at this temperature. The mixture is allowed to warm to 0° C. At about 0° C., the reaction mixture is poured into cold water, acidified using 10% HCl and extracted twice with methyl tert-butyl ether. The combined organic phases are washed with water, dried over Na2SO4 and filtered, and the solvent is removed under reduced pressure. The residue is filtered through SiO2 (heptane/dichloromethane 1:1), (yield: 17.6 g, 78%).

1. extractionextracted twice with methyl tert-butyl ether
2. washThe combined organic phases are washed with water
3. dry with materialdried over Na2SO4
4. filtrationfiltered
5. customthe solvent is removed under reduced pressure
6. filtrationThe residue is filtered through SiO2 (heptane/dichloromethane 1:1), (yield: 17.6 g, 78%)