HRID2266783

反应详情

EQUATION

反应方程式

HRID 2266783 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 (1H-imidazol-2-yl)-[1-phenyl-meth-(E)-ylidene]-amine (0.19 ml, 1.63 mmol) in toluene (6 ml) was added scandium triflate (59 mg, 0.12 mmol). An ethereal solution of ethylmagnesium bromide (0.97 ml, 3 M, 2.91 mmol) was then added dropwise and the reaction mixture was stirred at room temperature for 2 hours and then quenched by the addition of saturated aqueous ammonium chloride solution. The mixture was extracted twice with ether and the organic phases were dried over sodium sulfate and concentrated in vacuo. The residue was purified by chromatography on silica gel (eluant:methanol/dichloromethane 0:100 to 10:90) to yield the title compound as a brown gum (67 mg, 29%); MS (ISP): 202.4 ([M+H]+).

WORKUP

后处理

  1. customquenched by the addition of saturated aqueous ammonium chloride solution
  2. extractionThe mixture was extracted twice with ether
  3. dry with materialthe organic phases were dried over sodium sulfate
  4. concentrationconcentrated in vacuo
  5. customThe residue was purified by chromatography on silica gel (eluant:methanol/dichloromethane 0:100 to 10:90)