反应详情

温度

-10 °C

A solution of 5-[3-(4-Chloro-2-methyl-phenyl)-3-(3-fluoro-4-isopropoxy-phenyl)-propionyl]-1-methyl-1H-pyridin-2-one (example 323, step 4, 1.969 g) in dichloromethane (32.5 mL) was cooled to −10° C. At this temperature boron trichloride solution (1 M in dichloromethane, 13.4 mL) was slowly added. The reaction mixture was stirred at −10° C. for 1 h. The crude reaction mixture was poured into water/sat. sodium hydrogencarbonate-solution, extracted 3× with ethyl acetate, the organic layers were washed 2× with water, dried over magnesium sulfate and concentrated in vacuo to give the title compound as a light yellow solid, MS (ESI−): m/z=397.9 [M−H]−.

1. customThe crude reaction mixture
2. extractionsodium hydrogencarbonate-solution, extracted 3× with ethyl acetate
3. washthe organic layers were washed 2× with water
4. dry with materialdried over magnesium sulfate
5. concentrationconcentrated in vacuo