HRID1155855

反应详情

EQUATION

反应方程式

HRID 1155855 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
190 °C

PROCEDURE

实验过程

A mixture of 2-(3-methoxyphenyl)propyl 2-phenylethyl ether (176 mg., 0.65 mmole), pyridine (0.4 ml., 4.96 mmole) and dry pyridine hydrochloride (4 g., 34.6 mmole) is heated at 190° C. for 6 hours. The reaction mixture is cooled and added to a mixture of water (100 ml.) and ether (150 ml.). The ether extract is washed once with water (50 ml.) and, along with a second ether extract (50 ml.) of aqueous phase, is dried over magnesium sulfate and evaporated to an oil. The oil is purified via preparation layer chromatography on silica gel plates, eluted six times with 30% ether-pentane to yield the title product.

WORKUP

后处理

  1. temperatureThe reaction mixture is cooled
  2. extractionThe ether extract
  3. washis washed once with water (50 ml.) and, along with a second ether
  4. extractionextract (50 ml.) of aqueous phase
  5. dry with materialis dried over magnesium sulfate
  6. customevaporated to an oil
  7. customThe oil is purified via preparation layer chromatography on silica gel plates
  8. washeluted six times with 30% ether-pentane