HRID417041

反应详情

EQUATION

反应方程式

HRID 417041 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

Trifluoro-methanesulfonic acid 3-acetyl-5-trifluoromethanesulfonyloxy-phenyl ester (9.9 g) was dissolved in 1,2-dimethoxyethane (80 mL), followed by addition of cesium carbonate (11.6 g). The resulting suspension was stirred at 80° C. for 3 h and then quenched with saturated solution of ammonium chloride. The solution was then extracted with diethyl ether and combined etherate extracts were washed with brine, dried over anhydrous sodium sulfate, and filtered through a silica pad. The filtrate was concentrated under reduced pressure and purified on a silica gel column using ethyl acetate and hexanes to afford 3.5 g of the title compound (52% yield). HRMS calcd for C19H7O5S1F3 [M+H]+ 285.0039, observed 285.0039.

WORKUP

后处理

  1. customquenched with saturated solution of ammonium chloride
  2. extractionThe solution was then extracted with diethyl ether
  3. washwere washed with brine
  4. dry with materialdried over anhydrous sodium sulfate
  5. filtrationfiltered through a silica pad
  6. concentrationThe filtrate was concentrated under reduced pressure
  7. custompurified on a silica gel column