HRID1970047

反应详情

EQUATION

反应方程式

HRID 1970047 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

20 mg (0.11 mmol) of copper iodide, 28 mg (0.27 mmol) of triethylamine and 14 mg (0.02 mmol) of dichlorobis(triphenylphosphine)-palladium (II) are added to a suspension of 80 mg (0.21 mmol) of 8-iodo-4-oxo-4,5-dihydro-3H-pyrrolo[2,3-c]quinoline-1-ethyl carboxylate in 2.4 ml of anhydrous dioxan, then this mixture is degassed under argon. After 15 minutes, 32 mg (0.31 mmol) of phenylacetylene is added, then the mixture is heated at 100° C. for 3 hours. The raw reaction product is filtered on celite, the filtrate is evaporated to dryness and the residue is purified by chromatography on silica (eluent cyclohexane/ethyl acetate) to give 70 mg (93%) of 4-oxo-8-phenylethynyl-4,5-dihydro-3H-pyrrolo[2,3-c]quinoline-1-ethyl carboxylate in the form of a yellow solid.

WORKUP

后处理

  1. customthis mixture is degassed under argon
  2. customThe raw reaction product
  3. filtrationis filtered on celite
  4. customthe filtrate is evaporated to dryness
  5. customthe residue is purified by chromatography on silica (eluent cyclohexane/ethyl acetate)