HRID66927

反应详情

EQUATION

反应方程式

HRID 66927 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

A solution of alpha-hydroxyacetanilide (3.62 g, 0.024 mole), 4,4'-bis(N,N-dimethylamino)benzhydrol, methyl ether (6.81 g, 0.024 mole) 50 ml of tetrahydrofuran, 153 ml of n-hexane, and one drop of methanesulfonic acid was refluxed for 11 hours, during which time an additional 300 ml of solvent was added. The blue-green solution was decolorized with 4 drops of tetramethylguanidine and the reaction mixture was filtered hot and the filtrate chilled. Yellow-green crystals formed, which were recrystallized from 30 ml petroleum ether/15 ml acetone to give a white solid, mp 118°-128° C.

WORKUP

后处理

  1. additionwas added
  2. filtrationthe reaction mixture was filtered hot
  3. temperaturethe filtrate chilled
  4. customYellow-green crystals formed
  5. customwhich were recrystallized from 30 ml petroleum ether/15 ml acetone
  6. customto give a white solid, mp 118°-128° C.