HRID539495

反应详情

EQUATION

反应方程式

HRID 539495 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Water (0.25 ml) was added to the silica gel supporting scandium produced in Example 1 (75 mg), and while stirring, benzaldehyde (0.125 mmol) and o-anisidine (0.125 mmol) and 1-cyclohexenyloxytrimethylsilane (0.25 mmol) were continuously added. The mixture was stirred at room temperature for 24 hours. The mixture was extracted four times by a decantation method using a mixture of ethyl acetate-hexane (1:1), the solvent was distilled off under reduced pressure, and then the residue was purified by silica gel thin layer chromatography, to obtain the target product, 2-(phenyl-N-(2-methoxyphenyl)aminomethyl)cyclohexanone at a syn/anti ratio of 53/47. Yield 92%.

WORKUP

后处理

  1. stirringThe mixture was stirred at room temperature for 24 hours
  2. extractionThe mixture was extracted four times by a decantation method
  3. additiona mixture of ethyl acetate-hexane (1:1)
  4. distillationthe solvent was distilled off under reduced pressure
  5. customthe residue was purified by silica gel thin layer chromatography