HRID1383907

反应详情

EQUATION

反应方程式

HRID 1383907 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 4,4′-dichlorobenzhydryl chloride (5.20 g, 19.1 mmol) and 2-(methylamino)ethanol (9.0 g, 0.106 mol) in acetonitrile (100 ml) was treated with powdered anhydrous potassium carbonate (10 g) and the resulting mixture was heated under reflux for 4 h. The cooled mixture was filtered and the filtrate was concentrated in vacuo. The residual oil was diluted with ethyl acetate, washed with water and brine and then dried over anhydrous magnesium sulfate. Evaporation of the solvent in vacuo followed by chromatography on silica gel (elution toluene-ethyl acetate 9:1) gave 4.29 g (79%) of the title material as a white solid: mp 49-50° C.

WORKUP

后处理

  1. temperaturethe resulting mixture was heated
  2. temperatureunder reflux for 4 h
  3. filtrationThe cooled mixture was filtered
  4. concentrationthe filtrate was concentrated in vacuo
  5. additionThe residual oil was diluted with ethyl acetate
  6. washwashed with water and brine
  7. dry with materialdried over anhydrous magnesium sulfate
  8. customEvaporation of the solvent in vacuo