HRID355845

反应详情

EQUATION

反应方程式

HRID 355845 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of 0.90 g of N-(4-nitrobenzoyl)-N-(2-iodophenyl)-2-iodobenzeneethylamine in 10 ml of N,N-dimethylpropyleneurea (DMPU) is added 1.91 g of "activated" copper bronze. The mixture is stirred and heated at 195° for 2 days, cooled and slowly dropped into 100 ml of 0.5N HCl with stirring. The precipitate is filtered, washed with H2O and air dried (1.0 g of solid). The solid is extracted with ethyl acetate to give 0.50 g of solid. Chromatography on thick layer silica gel plates with ethyl acetate-hexane (1:2) as solvent gives 0.15 g of yellow solid.

WORKUP

后处理

  1. temperatureheated at 195° for 2 days
  2. temperaturecooled
  3. stirringwith stirring
  4. filtrationThe precipitate is filtered
  5. washwashed with H2O and air
  6. dry with materialdried (1.0 g of solid)
  7. extractionThe solid is extracted with ethyl acetate