HRID1460224

反应详情

EQUATION

反应方程式

HRID 1460224 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of α,α-bis(4-fluorophenyl)-4-piperidinemethanol (6.0 g, 0.02 mole), 4-(3-chloropropoxy)-3-methoxybenzoic acid methyl ester (5.4 g, 0.021 mole), anhydrous sodium carbonate (7.4 g, 0.07 mole), and potassium iodide (0.3 g) in 150 ml of dimethylformamide was heated on a steam bath for about 20 hr. The mixture was concentrated under reduced pressure, and the residue was partitioned between water and organic solvent (benzene). The organic layer was washed with water and brine and dried over sodium sulfate and eventually crystallized from 2-propanol to give the title compound as a white solid, mp 131°-132.5° C. (2-propanol).

WORKUP

后处理

  1. temperaturewas heated on a steam bath for about 20 hr
  2. concentrationThe mixture was concentrated under reduced pressure
  3. customthe residue was partitioned between water and organic solvent (benzene)
  4. washThe organic layer was washed with water and brine
  5. dry with materialdried over sodium sulfate
  6. customeventually crystallized from 2-propanol