HRID1860680

反应详情

EQUATION

反应方程式

HRID 1860680 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

In a flask equipped with a Dean-stark trap was prepared a solution of 1-(4-Methoxy-phenyl)-propan-2-one (40 g), ethyl cyanoacetate (27.56 g), ammonium acetate (9.40 g), acetic acid (14.64 g) and toluene (150 ml) at room temperature. The solution was heated to reflux overnight. The solution was cooled to room temperature, washed with water and brine, and concentrated. The crude product was purified on a silica gel column, eluting with 10% ethyl acetate/hexane to afford colorless oil (40.76 g). The 1H NMR was consistent with the proposed structure.

WORKUP

后处理

  1. customIn a flask equipped with a Dean-stark trap
  2. temperatureThe solution was heated
  3. temperatureto reflux overnight
  4. washwashed with water and brine
  5. concentrationconcentrated
  6. customThe crude product was purified on a silica gel column
  7. washeluting with 10% ethyl acetate/hexane