反应详情

温度

-78 °C

To a stirred solution of (2R,6S)-4-[6-({[tert-butyl(diphenyl)silyl]oxy}methyl)-2,3-difluorophenyl]-2,6-dimethylmorpholine (Intermediate 3, 1 g, 2.0 mmol) in anhydrous THF (10 mL), s-butyllithium (4.5 ml, 1.4M in cyclohexane, 6.3 mmol) was added and stirred for 2 h at −78° C. Benzaldehyde (685 mg, 0.0064 mmol) in THF (5 mL) was added dropwise and the solution was stirred for additional 1 h. The reaction mixture was quenched with saturated ammonium chloride solution and extracted with ethyl acetate. The organic layer was washed with brine and dried (Na2SO4), and solvent was removed. The residue was purified over a silica gel chromatography column using ethyl acetate-pet. ether gradient, providing the title compound.

1. stirringthe solution was stirred for additional 1 h
2. customThe reaction mixture was quenched with saturated ammonium chloride solution
3. extractionextracted with ethyl acetate
4. washThe organic layer was washed with brine
5. dry with materialdried (Na2SO4), and solvent
6. customwas removed
7. customThe residue was purified over a silica gel chromatography column