HRID2294142

反应详情

EQUATION

反应方程式

HRID 2294142 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 3-[4-(2-methoxyphenyl)piperazin-1-yl]propyl methanesulfonate (2 g, 6.06 mmol), 2-amino-N,N-dimethylbenzamide (1 g, 6.06 mmol), prepared as in Example 22, and potassium carbonate (2.1 g, 15 mmol) in 50 mL of acetonitrile was heated at reflux for 30 hours. The mixture was poured into water and extracted with ethyl acetate. The organic phase was dried (K2CO3) and concentrated. The residue was purified on silica gel by flash chromatography eluting with 6% methanol/methylene chloride to give 2-{3-[4-(2-methoxyphenyl)-piperazin-1-yl]propylamino}-N,N-dimethylbenzamide (1.5 g, 3.78 mmol).

WORKUP

后处理

  1. temperaturewas heated
  2. temperatureat reflux for 30 hours
  3. extractionextracted with ethyl acetate
  4. dry with materialThe organic phase was dried (K2CO3)
  5. concentrationconcentrated
  6. customThe residue was purified on silica gel by flash chromatography
  7. washeluting with 6% methanol/methylene chloride