HRID1156276

反应详情

EQUATION

反应方程式

HRID 1156276 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. temperatureThe reaction is heated
  2. temperatureto reflux for 31/2 hours
  3. filtrationfiltered while hot
  4. washAfter washing the salts with benzene
  5. customthe filtrate is removed in vacuo
  6. customto give a solid
  7. customThis solid is triturated several times with isopropyl ether and finally hexane