HRID1766350

反应详情

EQUATION

反应方程式

HRID 1766350 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Cyanoethylacetate (2.07 g, 18.3 mmol) and 4-cyanobenzaldehyde (2.40 g, 18.3 mmol) are dissolved in ethanol (125 ml) under an argon atmosphere. Piperidine (46.7 mg, 0.55 mmol) is added, and the reaction mixture is stirred for 2 hours at room temperature. An ethanol (300 ml) solution of Example 1A (5.00 g, 18.3 mmol) and additional piperidine (0.156 g, 1.83 mmol) is added, and the reaction mixture is stirred at reflux for 16 hours. The reaction mixture is concentrated in vacuo and chromatographed over silica get with cyclohexane/ethyl acetate mixtures to give a pale yellow oil.

WORKUP

后处理

  1. stirringthe reaction mixture is stirred
  2. temperatureat reflux for 16 hours
  3. concentrationThe reaction mixture is concentrated in vacuo
  4. customchromatographed over silica
  5. customget with cyclohexane/ethyl acetate
  6. customto give a pale yellow oil