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
CONDITIONS
反应条件
- 温度
- 0 °C
PROCEDURE
实验过程
In a nitrogen stream, triethylsilane (1.23 mL, 7.72 mmol) and a boron trifluoride-diethyl ether complex (0.88 mL, 5.48 mmol) were added to a solution of (2-benzyloxy-phenyl)-(4-methylsulfanylphenyl)-methanol (2.13 g, 6.3 mmol) in acetonitrile (15 mL) at −40° C. and the mixture solution was stirred at the same temperature for 1.5 hours and further at 0° C. for 30 minutes, and then water was added thereto and the mixture was extracted with methylene chloride. The organic layer was washed with a saturated sodium chloride aqueous solution and dried (anhydrous magnesium sulfate), and then the solvent was distilled under reduced pressure. The obtained residue was purified by silica gel column chromatography [developing solution=ethyl acetate:n-hexane (1:10)] to obtain the title compound (1.9 g, 95%).
WORKUP
后处理
- extractionthe mixture was extracted with methylene chloride
- washThe organic layer was washed with a saturated sodium chloride aqueous solution
- dry with materialdried (anhydrous magnesium sulfate)
- distillationthe solvent was distilled under reduced pressure
- customThe obtained residue was purified by silica gel column chromatography [developing solution=ethyl acetate:n-hexane (1:10)]