HRID82748

反应详情

EQUATION

反应方程式

HRID 82748 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

To a stirred solution of 4,7-dioxo-7-phenyl-heptanoic acid (3.57 mmol, 1.0 eq.) in acetic acid (10 ml) was added tert-butyl 4-aminobenzoate (1.05 eq., 3.75 mmol). The mixture was heated to 80° C. for 36 hours. The solvent was evaporated in vacuo and the crude residue purified by flash silica-gel chromatography. Gradient elution with ethyl acetate/hexane (0% to 50% ethyl acetate in hexane over 20 minutes) gave the semi-pure product after combination of the appropriate fractions and evaporation of the solvent in vacuo. The tan solid obtained was used without further purification, 59% yield.

WORKUP

后处理

  1. customThe solvent was evaporated in vacuo
  2. customthe crude residue purified by flash silica-gel chromatography
  3. washGradient elution with ethyl acetate/hexane (0% to 50% ethyl acetate in hexane over 20 minutes)
  4. customgave the semi-pure product
  5. customafter combination of the appropriate fractions and evaporation of the solvent in vacuo
  6. customThe tan solid obtained
  7. customwas used without further purification, 59% yield