HRID1821160

反应详情

EQUATION

反应方程式

HRID 1821160 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 the crude mixture of 4-(4-oxo-cyclohex-1-enyl)-benzonitrile and 4-(4-oxo-cyclohex-1-enyl)-benzonitrile prepared above in step c (36.6 mmol) in EtOAc (120 mL) was added 10% Pd—C (900 mg) and the reaction was degassed (3× vacuum and H2). After being stirred 7 hours under H2 atmosphere, additional 10% Pd—C (500 mg) was added and the resulting reaction was stirred for an additional 12 h under H2 atmosphere. The catalyst was removed by filtration through Celite and the filtrate was concentrated under reduced pressure to give 4-(4-oxo-cyclohexyl)-benzonitrile as a white solid. The product was used for next step without further purification.

WORKUP

后处理

  1. customthe reaction was degassed (3× vacuum and H2)
  2. additionadditional 10% Pd—C (500 mg) was added
  3. customthe resulting reaction
  4. stirringwas stirred for an additional 12 h under H2 atmosphere
  5. customThe catalyst was removed by filtration through Celite
  6. concentrationthe filtrate was concentrated under reduced pressure