HRID1432041
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
A solution of 4-chloro-1-(3-fluoro-phenylsulfanyl)-2-methoxybenzene (3.12 g, 11.6 mmol) in dry toluene (60 mL) was cooled to 0° C. Neat BBr3 (1.50 mL, 15.9 mmol) was added dropwise and the mixture was allowed to reach room temperature overnight. The mixture was quenched by the addition of H2O/ice (50 mL) and diethyl ether (50 mL). The aqueous layer was extracted with diethylether (2×50 mL). The combined organic layers were washed with brine, dried over Na2SO4 and adsorbed onto silica gel. After flash chromatography using silica gel, eluting with heptanes/EtOAc, 95:5, the title compound was obtained as a light yellow oil (2.26 g, 77%).
WORKUP
后处理
- customThe mixture was quenched by the addition of H2O/ice (50 mL) and diethyl ether (50 mL)
- extractionThe aqueous layer was extracted with diethylether (2×50 mL)
- washThe combined organic layers were washed with brine
- dry with materialdried over Na2SO4
- washeluting with heptanes/EtOAc, 95:5