HRID1820857
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
52.0 g (0.30 mol) of 2-chloro-4-nitrophenol is dissolved in 500 mL of DMF and 165 g (1.20 mol) of potassium carbonate is added batchwise. The mixture is stirred for 30 minutes at ambient temperature. Then 51.6 g (0.30 mol) of 2-diethylaminoethylchloride hydrochloride is added and the mixture is stirred for 3 days at ambient temperature. After this time, the mixture is filtered off, the solvent is eliminated, the residue is taken up in ethyl acetate, and washed with water. The organic phase is filtered through aluminum oxide (activity 2-3) and concentrated by evaporation. Yield: 41.0 g (50% of theory); Rf value: 0.60 (silica gel, methylene chloride/methanol/ammonia=9:1:0.01); C12H17ClN2O3.
WORKUP
后处理
- stirringthe mixture is stirred for 3 days at ambient temperature
- filtrationAfter this time, the mixture is filtered off
- washwashed with water
- filtrationThe organic phase is filtered through aluminum oxide (activity 2-3)
- concentrationconcentrated by evaporation