HRID859671

反应详情

EQUATION

反应方程式

HRID 859671 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 (4-bromo-2-ethyl-phenyl)-methanol (7.9 g, 36.7 mmol) in anhydrous CHCl3 (122 mL) was added PBr3(4.2 mL, 44.1 mmol). The resulting mixture was stirred at room temperature for 2 hours before it was quenched by the addition of water. The organic layer was washed with NaHCO3, brine and dried over MgSO4. The solvent was removed in vacuo and the residue was filtered through a pad of silica gel with 20% EtOAc in hexanes. The solvent was removed in vacuo to afford the desired product (8.4 g, 83%). 1H NMR (300 MHz, CDCl3): δ 1.29 (t, J=7.5 Hz, 3 H), 2.71–2.78 (m, 2 H), 4.48 (s, 2H), 7.17–7.20 (m, 1H), 7.29–7.32 (m, 1 H), 7.36–7.38 (m, 1H).

WORKUP

后处理

  1. customwas quenched by the addition of water
  2. washThe organic layer was washed with NaHCO3, brine
  3. dry with materialdried over MgSO4
  4. customThe solvent was removed in vacuo
  5. filtrationthe residue was filtered through a pad of silica gel with 20% EtOAc in hexanes
  6. customThe solvent was removed in vacuo