HRID2387749

反应详情

EQUATION

反应方程式

HRID 2387749 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

The compound 326-3 (4.78 g) was dissolved in toluene (130 ml). Cesium carbonate (10.6 g), 1,10-phenanthroline (4.41 g) and copper iodide (3.1 g) were added to the solution, and the obtained mixture was stirred for 5 minutes. Thereafter, benzyl alcohol (5.28 ml) was added to the reaction mixture. The obtained mixture was stirred at 110° C. for 5 days. The reaction mixture was diluted with ethyl acetate and filtered. The filtrate was concentrated under reduced pressure, and the obtained residue was purified by silica gel column chromatography (n-heptane:ethyl acetate=19:1 to 1:2), so as to obtain the title compound (1.42 g).

WORKUP

后处理

  1. stirringThe obtained mixture was stirred at 110° C. for 5 days
  2. filtrationfiltered
  3. concentrationThe filtrate was concentrated under reduced pressure
  4. customthe obtained residue was purified by silica gel column chromatography (n-heptane:ethyl acetate=19:1 to 1:2)