HRID1820857

反应详情

EQUATION

反应方程式

HRID 1820857 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. stirringthe mixture is stirred for 3 days at ambient temperature
  2. filtrationAfter this time, the mixture is filtered off
  3. washwashed with water
  4. filtrationThe organic phase is filtered through aluminum oxide (activity 2-3)
  5. concentrationconcentrated by evaporation