HRID650990

反应详情

EQUATION

反应方程式

HRID 650990 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

2,45 g of 2-[2-(N,N-dimethylamino)ethyl]oxy-benzoic acid are dissolved with 1.91 g of N-ethyl-N-dimethylaminopropyl)carbodiimide hydrochloride and catalytic amounts of hydroxybenzotriazole in 50 ml of DMF. After 15 minutes 1.52 g of 4-hydroxybenzoic acid amidoxime are added and the mixture is heated for 15 minutes at 700 W in the microwave. It is concentrated by evaporation, the residue is taken up in ethyl acetate, washed with water, dried over sodium sulphate and concentrated by evaporation in vacuo. The residue is filtered over silica gel with ethanol and converted into the salt as described above. Yield: 1.1 g (29% of theory). m.p.: 170° C. (decomposition).

WORKUP

后处理

  1. temperaturethe mixture is heated for 15 minutes at 700 W in the microwave
  2. concentrationIt is concentrated by evaporation
  3. washwashed with water
  4. dry with materialdried over sodium sulphate
  5. concentrationconcentrated by evaporation in vacuo
  6. filtrationThe residue is filtered over silica gel with ethanol