HRID82748
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- customThe solvent was evaporated in vacuo
- customthe crude residue purified by flash silica-gel chromatography
- washGradient elution with ethyl acetate/hexane (0% to 50% ethyl acetate in hexane over 20 minutes)
- customgave the semi-pure product
- customafter combination of the appropriate fractions and evaporation of the solvent in vacuo
- customThe tan solid obtained
- customwas used without further purification, 59% yield