HRID2115075

反应详情

EQUATION

反应方程式

HRID 2115075 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 0.9 g (4 mmol) of 2-chloro-N-(2-oxo-2,3-dihydro-1H-indol-5-yl)-acetamide, 0.7 g (4 mmol) of potassium iodide, 0.6 ml (4 mmol) of triethylamine, 0.53 ml (3 mmol) of 4-benzyl-piperidine and 50 ml of acetonitrile is refluxed for 20 hours. The reaction mixture is concentrated and 30 ml of water and 30 ml of chloroform are added to the residue. The organic layer is separated and the water phase is extracted three times with 10 ml of chloroform. The combined organic layers are dried over sodium sulfate, concentrated and the residue is treated with diethylether and the precipitated crystals are filtered off to yield 0.7 g (64%) of the title compound. Melting Point: 176-180° C. (diethylether)

WORKUP

后处理

  1. temperatureis refluxed for 20 hours
  2. concentrationThe reaction mixture is concentrated
  3. addition30 ml of water and 30 ml of chloroform are added to the residue
  4. customThe organic layer is separated
  5. extractionthe water phase is extracted three times with 10 ml of chloroform
  6. dry with materialThe combined organic layers are dried over sodium sulfate
  7. concentrationconcentrated
  8. additionthe residue is treated with diethylether
  9. filtrationthe precipitated crystals are filtered off