HRID2236565
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperaturethe reaction solution is heated at 60□C under N2 for 20 minutes
- customAfter evaporating to dryness
- dissolutionthe resulting brown residue is dissolved in methylene chloride
- washwashed twice with saturated Na2CO3 solution
- dry with materialAfter drying over Mg2SO4
- filtrationthe organic solution is filtered
- concentrationconcentrated