HRID1246960
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
- 0 °C
PROCEDURE
实验过程
A mixture of 1-phenylcyclobutanecarbonitrile (5 g) and acetic acid (15 ml) and H2SO4 (10 ml) and KNO3 (1.1 eq) was stirred at 0° C. for 20 min. The mixture was warmed to RT and stirred for two hours. The mixture was poured on ice and stirred until all ice melted. The precipitate was filtered and recrystalized from EtOH to give 1-(4-nitrophenyl)-cyclobutanecarbonitrile. The above product (2 g) was mixed with Pd—C (10%, 800 mg) in EtOH (100 ml) and hydrogenated under H2 atmosphere for 1 hour. The reaction was filtered through Celite and evaporated to give 1-(4-aminophenyl)-cyclobutanecarbonitrile, Mass: (M+1) 172, which was used for next step without further purification.
WORKUP
后处理
- temperatureThe mixture was warmed to RT
- stirringstirred for two hours
- additionThe mixture was poured on ice
- stirringstirred until all ice
- filtrationThe precipitate was filtered
- customrecrystalized from EtOH