HRID2286511

反应详情

EQUATION

反应方程式

HRID 2286511 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 3-methyl-1-bromo-butane (3.94 g.), N-nitroso-piperazine (3 g.), anhydrous potassium carbonate (3.6 g.) and a small crystal of potassium iodide in dimethyl formamide was heated at 100° for 2 hours. Solvent was removed under reduced pressure and the residue dissolved in ether and water. The ether extract was separated, dried and evaporated to give an oil which was adsorbed on silica gel. Elution with ethyl acetate gave N-(3-methylbutyl)-N'-nitroso piperazine, further purified by dissolving in dilute acid, washing the acid extract with ether, basifying the acid extract and re-extracting with ether. The yield of colourless oil was 3 g (62%).

WORKUP

后处理

  1. customSolvent was removed under reduced pressure
  2. dissolutionthe residue dissolved in ether
  3. extractionThe ether extract
  4. customwas separated
  5. customdried
  6. customevaporated
  7. customto give an oil which
  8. washElution with ethyl acetate