反応 #8906

反応方程式

product

3-Acetyl-6-(2-chlorophenyl)-5-(4-chlorophenyl)pyridin-2 (1H)-one

cesium carbonate

1-bromopinacolone

→

title compound

1-{[3-Acetyl-6-(2-chlorophenyl)-5-(4-chlorophenyl)pyridin-2-yl]oxy}-3,3-dimethylbutan-2-one

溶媒

DMF

反応条件

後処理

1. 1
   その他To a 25 mL rb flask equipped with a magnetic stir bar
2. 2
   workup.ADDITIONwas added
3. 3
   その他then partitioned between EtOAc and water
4. 4
   その他The organic layer was separated
5. 5
   洗浄washed with 10% aq. NaHSO4, water, brine
6. 6
   乾燥dried (MgSO4)
7. 7
   ろ過filtered
8. 8
   その他evaporated
9. 9
   その他The residue was purified on s silica gel flash chromatography column
10. 10
    洗浄eluted with 0–10% EtOAc-hexane
11. 11
    その他Evaporation of the purified fractions
12. 12
    その他drying in vacuo

実験手順

To a 25 mL rb flask equipped with a magnetic stir bar was added 0.309 g(0.86 mmol) of the product of Step A, 0.422 g (1.29 mmol) of cesium carbonate, 3 mL DMF and finally 145 μL of 1-bromopinacolone was added. The reaction mixture was stirred at room temperature for 1.5 h then partitioned between EtOAc and water. The organic layer was separated, washed with 10% aq. NaHSO4, water, brine, dried (MgSO4), filtered and evaporated. The residue was purified on s silica gel flash chromatography column eluted with 0–10% EtOAc-hexane. Evaporation of the purified fractions and drying in vacuo afforded the title compound.

出典