HRID1432041

反应详情

EQUATION

反应方程式

HRID 1432041 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. customThe mixture was quenched by the addition of H2O/ice (50 mL) and diethyl ether (50 mL)
  2. extractionThe aqueous layer was extracted with diethylether (2×50 mL)
  3. washThe combined organic layers were washed with brine
  4. dry with materialdried over Na2SO4
  5. washeluting with heptanes/EtOAc, 95:5