HRID513976

反应详情

EQUATION

反应方程式

HRID 513976 的结构方程式

PROCEDURE

实验过程

To the mixture of 6-methyl-hept-5-en-2-one (90.86 g, 0.72 mol) and benzyl cyanide (46.8 g, 0.40 mol) is added dropwise a 4 N solution of KOH in MeOH (25.0 ml, 0.10 mol). The resulting suspension is heated to reflux during 4.5 h. Then methanol is removed by distillation and the residue is washed with 6 N aq. HCl-solution, then water, sat. aq. NaHCO3-solution and brine. The organic layer is dried over MgSO4, the solvent removed under reduced pressure and the residue distilled twice over a Widmer column to yield 3,7-Dimethyl-2-phenyl-octa-2,6-diene nitrile (21.5 g, 24%, (E/Z) mixture) as a colourless oil (b.p. 122DC/0.1 mbar).

WORKUP

后处理

  1. temperatureThe resulting suspension is heated
  2. temperatureto reflux during 4.5 h
  3. customThen methanol is removed by distillation
  4. washthe residue is washed with 6 N aq. HCl-solution
  5. dry with materialThe organic layer is dried over MgSO4
  6. customthe solvent removed under reduced pressure
  7. distillationthe residue distilled twice over a Widmer column