HRID748683
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
The 2-[(4-chlorophenyl)sulfonylmethyl]-1,4-difluorobenzene (0.94 g, 3.1 mmol) obtained in Example 5 was dissolved in toluene (30 ml). After addition of 4-vinyloxy-1-butanol (0.51 ml, 4.2 mmol) and cyanomethylenetri-n-butylphosphorane (1.0 g, 4.1 mmol), the resulting mixture was heated under reflux for 3 days under an argon atmosphere. The reaction mixture was allowed to cool down and then concentrated under reduced pressure. The residue thus obtained was purified by silica gel chromatography (hexane:ethyl acetate=10:1) to yield a white solid. The resulting white solid was washed with hexane, whereby the title compound (0.97 g, 78%) was obtained as a white powder.
WORKUP
后处理
- temperaturethe resulting mixture was heated
- temperatureunder reflux for 3 days under an argon atmosphere
- temperatureto cool down
- concentrationconcentrated under reduced pressure
- customThe residue thus obtained
- customwas purified by silica gel chromatography (hexane:ethyl acetate=10:1)
- customto yield a white solid
- washThe resulting white solid was washed with hexane, whereby the title compound (0.97 g, 78%)
- customwas obtained as a white powder