HRID1899098
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
PROCEDURE
实验过程
A mixture of 5-acetyl-2-(4-fluorophenyl)-3-[4-(methylsulfonyl)phenyl]thiophene (1.8 g) and (triphenylphosphoranylidene)acetonitrile (3.2 g) in toluene (40 ml) was refluxed for 28 hours. The mixture was cooled and filtered. The filtrate was concentrated and the residue (4.2 g) was purified by column chromatography on silica gel eluting with a mixture of toluene and ethyl acetate (10:1). The obtained crystals (1.8 g) were recrystallized from ethanol to give colorless crystals of 3-{5-(4-fluorophenyl)-4-[4-(methylsulfonyl)phenyl]-2-thienyl}-2-butenenitrile (1.5 g).
WORKUP
后处理
- temperaturewas refluxed for 28 hours
- temperatureThe mixture was cooled
- filtrationfiltered
- concentrationThe filtrate was concentrated
- customthe residue (4.2 g) was purified by column chromatography on silica gel eluting with a mixture of toluene and ethyl acetate (10:1)
- customThe obtained crystals (1.8 g) were recrystallized from ethanol