HRID880472

反应详情

EQUATION

反应方程式

HRID 880472 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Benzyl bromide (0.6 mL, 5.04 mmol) was added dropwise to a mixture of 2-chloro-5-nitro-phenol (800 mg, 4.61 mmol) and potassium carbonate (1.27 g, 9.22 mmol) in acetone (20 mL) at ambient temperature and then heated at reflux for 2 h. The inorganic residue was filtered off and washed with acetone (20 mL). The combined filtrate and washings were concentrated in vacuo and the resulting residue was then dissolved in ethyl acetate (25 mL) and washed successively with water (2×20 mL), brine (20 mL), dried over anhydrous sodium sulfate and concentrated in vacuo to yield 2-benzyloxy-1-chloro-4-nitro-benzene (1.20 g, 99%) as a cream solid.

WORKUP

后处理

  1. temperatureheated
  2. temperatureat reflux for 2 h
  3. filtrationThe inorganic residue was filtered off
  4. washwashed with acetone (20 mL)
  5. concentrationThe combined filtrate and washings were concentrated in vacuo
  6. dissolutionthe resulting residue was then dissolved in ethyl acetate (25 mL)
  7. washwashed successively with water (2×20 mL), brine (20 mL)
  8. dry with materialdried over anhydrous sodium sulfate
  9. concentrationconcentrated in vacuo