HRID2403107

反应详情

EQUATION

反应方程式

HRID 2403107 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Small scale: Ethylene glycol (1 g, 16.1 mmol) was mixed with Triton B (40% in MeOH, 0.22 g, 0.53 mmol) and cooled in an ice-bath while acrylonitrile (1.71 g, 32.2 mmol) was added. The mixture was stirred at room temperature for 60 hours after which it was neutralized with 0.1M HCl (0.6 cm3) and extracted with CH2Cl2 (80 cm3). The extracts were concentrated under reduced pressure and the residue was Kugelrohr-distilled to give 3,3′-(ethane-1,2-diylbis(oxy))dipropanenitrile (1.08 g, 39.9%) as a light coloured oil, by 150-170° C./20 Torr.

WORKUP

后处理

  1. additionwas added
  2. extractionextracted with CH2Cl2 (80 cm3)
  3. concentrationThe extracts were concentrated under reduced pressure
  4. distillationthe residue was Kugelrohr-distilled