HRID620733

反应详情

EQUATION

反应方程式

HRID 620733 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

7-Nitro-1,2,4,5-tetrahydro-3H-3-benzazepine (0.7 g), 2-bromomethyl-5-nitrobenzofuran (0.93 g) and potassium carbonate (0.5 g) in acetonitrile were heated under reflux for 8 hours. After cooling the solvent was removed in vacuo, the residue dissolved in methylene chloride and washed three times with aqueous sodium carbonate and three times with brine. The organic layer was dried (Na2SO4) and evaporated in vacuo to give an oil methylene chloride. The product-containing fractions were combined and evaporated in vacuo to give an oil which was triturated with hexane and the evaporated in vacuo to give the title compound as a foam, yield 0.76 g.

WORKUP

后处理

  1. temperatureunder reflux for 8 hours
  2. temperatureAfter cooling the solvent
  3. customwas removed in vacuo
  4. dissolutionthe residue dissolved in methylene chloride
  5. washwashed three times with aqueous sodium carbonate and three times with brine
  6. dry with materialThe organic layer was dried (Na2SO4)
  7. customevaporated in vacuo
  8. customto give an oil methylene chloride
  9. customevaporated in vacuo
  10. customto give an oil which
  11. customwas triturated with hexane
  12. customthe evaporated in vacuo