HRID475695
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- customthe reaction was degassed (3×vacuum and H2)
- additionadditional 10% Pd—C (500 mg) was added
- customthe resulting reaction
- stirringwas stirred for an additional 12 h under H2 atmosphere
- customThe catalyst was removed by filtration through Celite
- concentrationthe filtrate was concentrated under reduced pressure