HRID1082135

反应详情

EQUATION

反应方程式

HRID 1082135 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A two-phase mixture of phenol (5 g, 53 mmol), dichloropropane (32 ml), tetrabutylammonium hydrogen sulphate (0.3 g, 1 mmol), and sodium hydroxide solution (25 ml, 3M) was refluxed for 3 h. The organic layer was separated, dried (MgSO4), washed through a plug of silica with dichloromethane (200 ml), and concentrated in vacuo. The residues were distilled to give the title compound as a colourless, viscous oil (8.0 g, 88%) bp 110° C. at 0.1 mm Hg. NMR (CDCl3, 250 MHz) δ=2.26 (2H,q,J=6 Hz), 3.77 (2H,t,J=6 Hz), 4.13 (2H,t,J=6 Hz), 6.90-7.00 (3H,m), 7.26-7.34 (2H,m).

WORKUP

后处理

  1. temperaturewas refluxed for 3 h
  2. customThe organic layer was separated
  3. dry with materialdried (MgSO4)
  4. washwashed through a plug of silica with dichloromethane (200 ml)
  5. concentrationconcentrated in vacuo
  6. distillationThe residues were distilled