HRID63922

反应详情

EQUATION

反应方程式

HRID 63922 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 1-(3-chlorophenyl)-3-(4-chlorophenyl)propan-1-one (1.39 g, 5 mmol) in HOAc (15 mL) at 0° C. was added Br2 (800 mg, 5 mmol) dropwise. The reaction was refluxed for 8 h, cooled to RT, concentrated then diluted with EA (25 mL) and water (5 mL). The organic layer was washed with brine (5 mL), dried over Na2SO4 and concentrated to give a residue which was purified by chromatography eluted with PE/EA (50:1) to give 2-bromo-1-(3-chlorophenyl)-3-(4-chlorophenyl)propan-1-one (358 mg, 20% yield) as a brown solid. LCMS: MH+ 359 and TR=2.029 min.

WORKUP

后处理

  1. temperatureThe reaction was refluxed for 8 h
  2. concentrationconcentrated
  3. additionthen diluted with EA (25 mL) and water (5 mL)
  4. washThe organic layer was washed with brine (5 mL)
  5. dry with materialdried over Na2SO4
  6. concentrationconcentrated
  7. customto give a residue which
  8. customwas purified by chromatography
  9. washeluted with PE/EA (50:1)