HRID620734

反应详情

EQUATION

反应方程式

HRID 620734 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 (0.35 g), 2-chloromethyl-6-nitroquinoline (0.4 g - see Chem. Pharm. Bull, 28, page 2441 [1980]), sodium iodide (0.27 g) and potassium carbonate (0.25 g) in acetonitrile were heated under reflux for 18 hours. The solvent was then removed in vacuo, the residue dissolved in methylene chloride and washed three times with aqueous sodium carbonate and twice with brine. The organic layer was dried (Na2SO4) and evaporated in vacuo to give an oil which was triturated with hexane to give the title compound, yield 0.61 g, m.p. 127°-130°.

WORKUP

后处理

  1. temperatureunder reflux for 18 hours
  2. customThe solvent was then removed in vacuo
  3. dissolutionthe residue dissolved in methylene chloride
  4. washwashed three times with aqueous sodium carbonate
  5. dry with materialThe organic layer was dried (Na2SO4)
  6. customevaporated in vacuo
  7. customto give an oil which
  8. customwas triturated with hexane