HRID2236565

反应详情

EQUATION

反应方程式

HRID 2236565 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 3-nitrobenzyl bromide (10.5 g, 48.7 mmol) in methylene chloride is added azepane (5.5 mL, 48.7 mmol) and 20.0 mL (146.1 mmol) of triethylamine, and the reaction solution is heated at 60□C under N2 for 20 minutes. After evaporating to dryness, the resulting brown residue is dissolved in methylene chloride and washed twice with saturated Na2CO3 solution, and once with brine solution. After drying over Mg2SO4, the organic solution is filtered and concentrated to give 8.0 g (70.1% yield) of brown oil.

WORKUP

后处理

  1. temperaturethe reaction solution is heated at 60□C under N2 for 20 minutes
  2. customAfter evaporating to dryness
  3. dissolutionthe resulting brown residue is dissolved in methylene chloride
  4. washwashed twice with saturated Na2CO3 solution
  5. dry with materialAfter drying over Mg2SO4
  6. filtrationthe organic solution is filtered
  7. concentrationconcentrated