HRID1822331

反应详情

EQUATION

反应方程式

HRID 1822331 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

A −78° C. solution of the crude 2-phenoxy-5-trifluoromethyl-anisole (3.79 g, 14.1 mmol) in CH2Cl2 (38 mL) is treated with BBr3 (14.04 g, 56.1 mmol) and then warmed to 0° C. The mixture is stirred for 1.5 h under N2, poured into ice water and extracted with Et2O. The organic layer is dried (Na2SO4), and the solvent is removed in vacuo to afford crude material that is absorbed on silica gel and columned with 6/1 hexanes/ethyl acetate to afford 1.29 g (18%) of the title compound. 1H NMR (400 MHz, CDCl3); MS (ES−+) m/z mass calculated for C13H9O2F3 254, found 253 (M+1, 100%).

WORKUP

后处理

  1. extractionextracted with Et2O
  2. dry with materialThe organic layer is dried (Na2SO4)
  3. customthe solvent is removed in vacuo
  4. customto afford crude material that
  5. customis absorbed on silica gel