반응 #82545

반응 방정식

1-fluoro-1-phenylsulfonyl-3-methyl-3-(4-chlorophenyl)-1-butene

tributyltin hydride

azobisisobutyronitrile

→

1-fluoro-3-(4-chlorophenyl)-3-methyl-1-tributylstannyl-1-butene

용매

cyclohexane

반응 조건

후처리

1. 1
   온도at reflux for about three hours
2. 2
   workup.ADDITION125 mL of silica gel is added
3. 3
   농축The mixture is concentrated under reduced pressure
4. 4
   농축concentrated under reduced pressure

실험 절차

Under a nitrogen atmosphere, a stirring solution of 22.7 grams (0.067 mole) of 1-fluoro-1-phenylsulfonyl-3-methyl-3-(4-chlorophenyl)-1-butene, 42.0 grams (0.14 mole) of tributyltin hydride, and 0.5 gram (catalyst) of azobisisobutyronitrile in 700 mL of cyclohexane is heated at reflux for about three hours. After this time the reaction mixture is cooled to ambient temperature, and 125 mL of silica gel is added. The mixture is concentrated under reduced pressure, and the residue is subjected to column chromatography. The product-containing fractions are combined and concentrated under reduced pressure, yielding 1-fluoro-3-(4-chlorophenyl)-3-methyl-1-tributylstannyl-1-butene.

출처