HRID2305239

反应详情

EQUATION

反应方程式

HRID 2305239 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 {3-{[2-(4,5-diphenyloxazol-2-yl)-2-cyclohexen-1-yl]methyl}phenyl}carbamic acid tert-butyl ester (2.34 g, 4.62 mmol) in methylene chloride (25 ml) was added trifluoroacetic acid (7 ml) at 5° C. and the mixture was stirred at room temperature for 1.5 hour. After evaporation, the residue was dissolved in EtOAc, and saturated sodium hydrogencarbonate solution was added thereto under ice-cooling. The mixture was extracted with EtOAc, washed with water and brine, dried over magnesium sulfate, and evaporated in vacuo. The residue was purified by silica gel column chromatography (hexane:EtOAc, 3:1 elution) to give 3-{[2-(4,5-diphenyloxazol-2-yl)-2-cyclohexen-1-y]methyl}phenylamine (1.74 g, 93%).

WORKUP

后处理

  1. customAfter evaporation
  2. dissolutionthe residue was dissolved in EtOAc
  3. additionsaturated sodium hydrogencarbonate solution was added
  4. temperatureunder ice-cooling
  5. extractionThe mixture was extracted with EtOAc
  6. washwashed with water and brine
  7. dry with materialdried over magnesium sulfate
  8. customevaporated in vacuo
  9. customThe residue was purified by silica gel column chromatography (hexane:EtOAc, 3:1 elution)