HRID1163289

反应详情

EQUATION

反应方程式

HRID 1163289 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

A mixture of phosphorus(V) oxide (10 g) and methanesulfonic acid (70 mL) was stirred at 100° C. for 1 hr. The obtained solution and 5-(3-methoxyphenyl)pentanoic acid (5.28 g, 25.4 mmol) were mixed and the mixture was stirred for 1 hr. The reaction mixture was poured into iced water and extracted with ethyl acetate. The extract was washed with saturated brine, dried over anhydrous magnesium sulfate and concentrated under reduced pressure. The residue was purified by silica gel column chromatography (hexane-30% ethyl acetate/hexane) to give the title compound (4.02 g, 83%) as a red-brown oil.

WORKUP

后处理

  1. stirringthe mixture was stirred for 1 hr
  2. extractionextracted with ethyl acetate
  3. washThe extract was washed with saturated brine
  4. dry with materialdried over anhydrous magnesium sulfate
  5. concentrationconcentrated under reduced pressure
  6. customThe residue was purified by silica gel column chromatography (hexane-30% ethyl acetate/hexane)