HRID377047

反应详情

EQUATION

反应方程式

HRID 377047 的结构方程式

CONDITIONS

反应条件

温度
150 °C

PROCEDURE

实验过程

622 g (4.5 mol) of isophorone and 1.8 g (12.9 mmol) of 1,3-dimethylimidazolium-4-carboxylate were placed in a reaction vessel and a mixture of 207.3 g (1.5 mol) of isophorone and 81.0 g (3 mol) of hydrogen cyanide was added at 150° C. over a period of about 60 minutes. The mixture was subsequently stirred further for about 60 minutes at 150° C. After cooling, the HCN concentration was determined by titration. No free hydrocyanic acid could be detected (HCN conversion>99.9%). After addition of 2.0 g of 85% strength H3PO4, the reaction product was distilled at 0.1 hPa. This gave 486 g of 3-cyano-3,5,5-trimethylcyclohexanone (98.1% based on HCN used). The amount of distillation residue was only 3% by weight, based on isophorone used.

WORKUP

后处理

  1. additionwas added at 150° C. over a period of about 60 minutes
  2. temperatureAfter cooling
  3. concentrationthe HCN concentration
  4. additionAfter addition of 2.0 g of 85% strength H3PO4
  5. distillationthe reaction product was distilled at 0.1 hPa
  6. distillationThe amount of distillation residue