HRID2042624

反应详情

EQUATION

反应方程式

HRID 2042624 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

In a 1 L round bottom flask, 4-(4-methoxyphenyl)-4-oxo-butyric acid (25 g, 106 mmol) in 48% HBr (125 mL) and acetic acid (250 mL) was heated to reflux 18 h. The reaction was cooled slightly and ethanol (250 mL) was added. The solvent was concentrated under vacuum. Additional ethanol (100 mL) was added and solvent concentrated under vacuum again. The resulting oil was crystallized from ethyl acetate/hexanes to produce 8.65 g (37%). MS m/z=223 (M+H).

WORKUP

后处理

  1. temperatureto reflux 18 h
  2. temperatureThe reaction was cooled slightly
  3. concentrationThe solvent was concentrated under vacuum
  4. additionAdditional ethanol (100 mL) was added
  5. concentrationsolvent concentrated under vacuum again
  6. customThe resulting oil was crystallized from ethyl acetate/hexanes
  7. customto produce 8.65 g (37%)