HRID1154643

反应详情

EQUATION

反应方程式

HRID 1154643 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

22 gm (0.075 mol) of N-[3-(7,8-dimethoxy-1,3,4,5-tetrahydro-2H-3-benzazepin-2-on-3-yl)-propyl]-methylamine were heated with 7.2 gm (0.036 mol) of 2-(3,4-dimethoxyphenyl)-ethyl-chloride for 20 hours at 140° C. After dissolving the reaction product in methylene chloride, the solution was washed twice with 2N sodium hydroxide and twice with water, dried over sodium sulfate and evaporated. The residue was purified by chromatography on silica gel (particle size: 0.063-0.2 mm; eluant; methylene chloride/methanol=10:1). The product thus obtained was dissolved in acetone, and the dihydrocyloride was precipitated with ethereal hydrochloric acid.

WORKUP

后处理

  1. washthe solution was washed twice with 2N sodium hydroxide and twice with water
  2. dry with materialdried over sodium sulfate
  3. customevaporated
  4. customThe residue was purified by chromatography on silica gel (particle size: 0.063-0.2 mm; eluant; methylene chloride/methanol=10:1)
  5. customThe product thus obtained
  6. customthe dihydrocyloride was precipitated with ethereal hydrochloric acid