HRID1269947
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
CONDITIONS
反应条件
- 温度
- 100 °C
PROCEDURE
实验过程
Under a nitrogen atmosphere, ammonium chloride (4.17 g, 0.078 mol) and potassium cyanide (6.77 g, 0.104 mol) were added to a solution of 2-cyclohexen-1-one (5.0 g, 0.052 mol) in a 15%-aqueous N,N-dimethylformamide solution (60 ml) at room temperature, and the resulting mixture was heated to 100° C. After 3 hours, the reaction solution was poured into water and extracted with chloroform, and the organic layer was dried over anhydrous magnesium sulfate. The organic layer dried was concentrated under reduced pressure and the resulting residue was purified by a silica gel column chromatography (eluent: hexane/ethyl acetate) to obtain 1-cyanocyclohexan-3-one (345.4 mg, 5.4%).
WORKUP
后处理
- extractionextracted with chloroform
- dry with materialthe organic layer was dried over anhydrous magnesium sulfate
- customThe organic layer dried
- concentrationwas concentrated under reduced pressure
- customthe resulting residue was purified by a silica gel column chromatography (eluent: hexane/ethyl acetate)