HRID1396058

反应详情

EQUATION

反应方程式

HRID 1396058 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

2.54 g 3-Bromo-5-chloro-phenol was dissolved in 50 mL acetone. Subsequently were added 8.04 g potassium carbonate, 1.52 mL benzyl bromide and 0.86 g tetrabutylammonium iodide. The mixture was refluxed for 2 h., cooled to room temperature and filtrated, and the filtrate was concentrated to dryness. The residue was chromatographed over a short column of silica, eluting with DCM/PA 1:4, and the pink color of the product fractions (at the front) was removed with active carbon. After filtration and evaporation, 3.11 g (90%) of a pale yellow oil was obtained. 1H NMR (400 MHz, CDCl3) δ 5.03 (s, 2H), 6.92 (t, J=2 Hz, 1H), 7.03 (t, J=2 Hz, 1H), 7.12 (t, J=1.5 Hz, 1H), 7.31-7.45 (m, 5H).

WORKUP

后处理

  1. temperatureThe mixture was refluxed for 2 h.
  2. filtrationfiltrated
  3. concentrationthe filtrate was concentrated to dryness
  4. customThe residue was chromatographed over a short column of silica
  5. washeluting with DCM/PA 1:4
  6. customthe pink color of the product fractions (at the front) was removed with active carbon
  7. filtrationAfter filtration and evaporation