反応 #8919

反応方程式

product

6-(2-chlorophenyl)-5-(4-chlorophenyl)-3-[(1-methyl-1H-imidazol-2-yl)carbonyl]pyridin-2 (1H)-one

1-bromopinacolone

Cs2CO3

→

title compound

1-({6-(2-Chlorophenyl)-5-(4-chlorophenyl)-3-[(1-methyl-1H-imidazol-2-yl)carbonyl]pyridin-2-yl}oxy)-3,3-dimethylbutan-2-one

溶媒

DMF

反応条件

後処理

1. 1
   その他partitioned between EtOAc and saturated aqueous NaHCO3 solution
2. 2
   その他The organic layer was separated
3. 3
   洗浄washed with aq. NaHCO3, brine
4. 4
   乾燥dried (Na2SO4)
5. 5
   ろ過filtered
6. 6
   その他evaporated
7. 7
   その他The residue was purified on a silica gel flash chromatography column
8. 8
   洗浄eluted with 0–75% EtOAc-hexane
9. 9
   その他Evaporation of the purified fractions
10. 10
    その他drying in vacuo

実験手順

To a solution of the product of Step A in 4 mL DMF was added 0.125 g (0.698 mmol) of 1-bromopinacolone and 0.455 g (1.39 mmol) of Cs2CO3. The reaction mixture was stirred at room temperature for 1 h, then partitioned between EtOAc and saturated aqueous NaHCO3 solution. The organic layer was separated, washed with aq. NaHCO3, brine, dried (Na2SO4), filtered and evaporated. The residue was purified on a silica gel flash chromatography column eluted with 0–75% EtOAc-hexane. Evaporation of the purified fractions and drying in vacuo afforded the title compound.

出典