HRID988966

反应详情

EQUATION

反应方程式

HRID 988966 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
110 °C

PROCEDURE

实验过程

To the solution of 2-ethyl-1-(hydroxyimino)cyclohexane (6.8 g, 48.5 mmol) in ethanol (75 mL) were added sodium pieces (about 8.0 g) in portions, and the reaction was heated to reflux at 110° C. overnight. More sodium pieces were added, and the reaction was stirred for another 6 hours. The reaction was treated with concentrated HCl (12 M, 4.0 mL) in water (25 mL). Ethanol was removed in vacuo. The aqueous layer was washed with ether (10 mL), and treated with aqueous KOH (25 mL) and extracted with ether (3×20 mL). The combined organic extracts were washed with brine (20 mL), dried over sodium sulfate, and concentrated in vacuo to give 2-ethylcyclohexylamine as an off-white oil.

WORKUP

后处理

  1. temperaturethe reaction was heated
  2. customEthanol was removed in vacuo
  3. washThe aqueous layer was washed with ether (10 mL)
  4. additiontreated with aqueous KOH (25 mL)
  5. extractionextracted with ether (3×20 mL)
  6. washThe combined organic extracts were washed with brine (20 mL)
  7. dry with materialdried over sodium sulfate
  8. concentrationconcentrated in vacuo