HRID1755776

反应详情

EQUATION

反应方程式

HRID 1755776 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

A mixture of the allylic alcohol of Step 3 (1.214 g, 3.75 mmol), 1-chloro-2-iodobenzene (480 FtL), Pd(OAc)2 (30 mg), LiCl (194 mg), LiOAc.2H2O (995 rag) and Bu4NCI (2.13 g) in 7.5 mL of DMF was degassed under vacuum and heated to 100° C. under N2 for 3 hr. 25% Aq. NH4OAc was then added and the product was extracted in EtOAc, dried over Na2SO4, and purified by flash chromatography with EtOAc: toluene 2.5:97.5. Yield 1.53 g, 94%.

WORKUP

后处理

  1. customwas degassed under vacuum
  2. addition25% Aq. NH4OAc was then added
  3. extractionthe product was extracted in EtOAc
  4. dry with materialdried over Na2SO4
  5. custompurified by flash chromatography with EtOAc: toluene 2.5:97.5