HRID66930

反应详情

EQUATION

反应方程式

HRID 66930 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of 4,4'-bis(N,N-dimethylamino)benzhydrol, methyl ether (11.0 g, 0.039 mole), benzyl glycolate (6.6 g, 0.039 mole), 90 ml of tetrahydrofuran, 200 ml of hexane, and 10 drops of methanesulfonic acid was refluxed for 6 hours, replacing solvent as distillate was removed; then, 10 drops of tetramethylguanidine was added to discharge the color and the reaction mixture was filtered hot and cooled. A white solid formed which was filtered, washed with petroleum ether and then recrystallized from 4/1 hexane/acetone. The resulting white crystalline product had a mp 101.8°-103° C.

WORKUP

后处理

  1. customwas removed
  2. additionthen, 10 drops of tetramethylguanidine was added
  3. filtrationthe reaction mixture was filtered hot
  4. temperaturecooled
  5. customA white solid formed which
  6. filtrationwas filtered
  7. washwashed with petroleum ether
  8. customrecrystallized from 4/1 hexane/acetone