HRID364075

反应详情

EQUATION

反应方程式

HRID 364075 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Here, 3-(7,8-dimethoxy-1,3,4,5-tetrahydro-2H-3-benzazepin-2-on-3-yl)-1-chloropropane (18.5 g, 0.0623 mol) is heated to 110° C. for 2 hours in an autoclave with N-(2-phenyloxyethyl)-methylamine (10.3 g, 0.0623 mol) and triethylamine (8.7 ml, 0.062 mol). After cooling, the reaction mixture is distributed between methylene chloride and water, the organic phase is separated off, dried over sodium sulfate and concentrated by evaporation. The residue is purified by chromatography on silica gel (eluant: methylene chloride/methanol=9/1). The base thus obtained is converted into the hydrochloride in the usual way.

WORKUP

后处理

  1. temperatureAfter cooling
  2. customthe organic phase is separated off
  3. dry with materialdried over sodium sulfate
  4. concentrationconcentrated by evaporation
  5. customThe residue is purified by chromatography on silica gel (eluant: methylene chloride/methanol=9/1)
  6. customThe base thus obtained