反应详情

温度

40 °C

A mixture of 69 mg (1.7 mmol) NaH (55% suspension in mineral oil), 359 mg (1.08 mmol) (S)-1-[(3S,4S)-1-benzyl-3-(4-chloro-phenyl)-piperidin-4-yl]-ethanol and 225 mg (1.52 mmol) 2,5-dichloropyridine in 2 mL DMF was stirred for 20 h at 40° C. Further 0.2 eq. 2,5-dichloropyridine was added and stirring was continued for 20 h at 60° C. After evaporation the residue was purified by column chromatography on silica eluting with a gradient formed from ethyl acetate and heptane to afford after evaporation of the product containing fractions 205 mg (43%) of the title compound as colorless viscous oil. MS (m/e): 441.1 [(M+H)+]

1. stirringstirring
2. waitwas continued for 20 h at 60° C
3. customAfter evaporation the residue
4. customwas purified by column chromatography on silica eluting with a gradient
5. customformed from ethyl acetate and heptane
6. customto afford
7. customafter evaporation of the product
8. additioncontaining fractions 205 mg (43%) of the title compound as colorless viscous oil