HRID1739811

反应详情

EQUATION

反应方程式

HRID 1739811 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Imidazole (121.8 g) was added to a mixture of 1-(chlorophenylmethyl)-4-nitrobenzene (88.7 g) in ACN (1000 ml) and the reaction mixture was stirred and refluxed for 24 hours. The solvent was evaporated. The residue was dissolved in toluene, washed with a 10% K2CO3 solution, dried (MgSO4), filtered and evaporated. The residue was purified by column chromatography over silica gel (eluent: CH2Cl2 /CH3OH 98/2). The pure fractions were collected and the solvent was evaporated, yielding 53 g (53%) of 1-[(4-nitrophenyl)phenylmethyl]-1H-imidazole (interm. 1-a).

WORKUP

后处理

  1. temperaturerefluxed for 24 hours
  2. customThe solvent was evaporated
  3. dissolutionThe residue was dissolved in toluene
  4. washwashed with a 10% K2CO3 solution
  5. dry with materialdried (MgSO4)
  6. filtrationfiltered
  7. customevaporated
  8. customThe residue was purified by column chromatography over silica gel (eluent: CH2Cl2 /CH3OH 98/2)
  9. customThe pure fractions were collected
  10. customthe solvent was evaporated