HRID1156276
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
11-Chloro-6,11-dihydrodibenz[b,e]oxepin (32.69 g; 0.14 mole) is dissolved in dry benzene (300 ml) and placed under a dry nitrogen atmosphere. To this solution is added in one portion, CuCN (32.04 g; 0.35 mole). The reaction is heated to reflux for 31/2 hours and filtered while hot. After washing the salts with benzene, the filtrate is removed in vacuo to give a solid. This solid is triturated several times with isopropyl ether and finally hexane to give a solid (92%) of 11-cyano-6,11-dihydrodibenz[b,e]oxepin m.p. 65°-66.5° C.
WORKUP
后处理
- temperatureThe reaction is heated
- temperatureto reflux for 31/2 hours
- filtrationfiltered while hot
- washAfter washing the salts with benzene
- customthe filtrate is removed in vacuo
- customto give a solid
- customThis solid is triturated several times with isopropyl ether and finally hexane