HRID736281

反应详情

EQUATION

反应方程式

HRID 736281 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

N′-Benzhydrylidene-N-(4-chlorophenyl)-N-methylhydrazine (1.5 g, 4.68 mmol) is placed in 20 mL of tetrahydrofuran with stirring. 5 mL of 5 N hydrochloric acid are added thereto and the solution is then left stirring at a temperature in the region of 50° C. for 16 hours. The aqueous phase is then neutralized with 5 N sodium hydroxide and is then extracted with ethyl acetate. The oil obtained after extraction is purified by chromatography on silica gel, eluting at the start with an ethyl acetate/heptane mixture (10/90 by volume). N-(4-Chlorophenyl)-N-methylhydrazine is thus obtained in the form of a pale yellow oil, 0.53 g (72%). (Rf=0.48. 20/80 EtOAc/heptane (v/v)).

WORKUP

后处理

  1. waitthe solution is then left
  2. stirringstirring at a temperature in the region of 50° C. for 16 hours
  3. extractionis then extracted with ethyl acetate
  4. customThe oil obtained
  5. extractionafter extraction
  6. customis purified by chromatography on silica gel
  7. washeluting at the start with an ethyl acetate/heptane mixture (10/90 by volume)