HRID1591748

反应详情

EQUATION

反应方程式

HRID 1591748 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 1.47 g (8.41 mmol) of 4-cyanophenylpropionic acid, 3.1 g (9.65 mmol) of TBTU and 5.0 ml of triethylamine in 150 ml of tetrahydrofuran was stirred at room temperature for 30 minutes, 2.5 g (8.41 mmol) of N-(3-aminopropyl)-2,3-dichloro-N-methylbenzenesulphonamide were than added and the mixture was stirred overnight. The mixture was evaporated to dryness, potassium carbonate solution (10%) was added to the residue and the mixture was extracted with ethyl acetate. The organic phase was washed with water and saturated sodium chloride solution, drive over sodium sulphate and concentrated. The crude product obtained in this manner was purified by column chromatography (mobile phase: dichloromethane/methanol 150:1 to 100:1).

WORKUP

后处理

  1. additionthan added
  2. customThe mixture was evaporated to dryness, potassium carbonate solution (10%)
  3. additionwas added to the residue
  4. extractionthe mixture was extracted with ethyl acetate
  5. washThe organic phase was washed with water and saturated sodium chloride solution, drive over sodium sulphate
  6. concentrationconcentrated