HRID1282062

反应详情

EQUATION

反应方程式

HRID 1282062 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of aluminum lithium hydride (2.1 g) in tetrahydrofuran (20 ml) was added a solution of ethyl 4-cyanomesitylenate (2.9 g) in tetrahydrofuran (30 ml) at 0° C. and the mixture was refluxed under heating for 6 hr. To this reaction mixture was added 50% (v/v) tetrahydrofuran in water under ice-cooling. This mixture was stirred at room temperature for 30 min and the catalyst was filtered off using Celite. The solvent was evaporated and the obtained residue was recrystallized from methanol-isopropyl ether to give the title compound (5.5 g) as white crystals.

WORKUP

后处理

  1. temperaturethe mixture was refluxed
  2. temperatureunder heating for 6 hr
  3. temperaturecooling
  4. filtrationthe catalyst was filtered off
  5. customThe solvent was evaporated
  6. customthe obtained residue was recrystallized from methanol-isopropyl ether