HRID734299

反应详情

EQUATION

反应方程式

HRID 734299 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 0.356 g (1.26 mmol) of N-[2-(3-indolyl)ethyl)]decahydroiso-quinoline in 20 ml of ethanol was added a solution of 1.6 g of mercuric acetate and 1.88 g of ethylenediaminetetra-acetic acid disodium salt dihydrate in 40 ml of water and the resulting mixture was refluxed for 3 h. The cooled mixture was made basic with dilute ammoniumhydroxide (pH 11) and then extracted with dichloromethane (3×30 ml). The combined organic layers were dried over sodium sulfate, filtered and the solvent evaporated to give the crude enamine (mixture of regioisomers), which was directly used in the next step (see example 36). The pure enamine could be obtained by column chromatography (silica gel, dichloromethane/methanol/triethylamine, 98:1:1).

WORKUP

后处理

  1. temperaturethe resulting mixture was refluxed for 3 h
  2. extractionextracted with dichloromethane (3×30 ml)
  3. dry with materialThe combined organic layers were dried over sodium sulfate
  4. filtrationfiltered
  5. customthe solvent evaporated
  6. customto give the crude enamine (mixture of regioisomers), which