HRID1755776
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
- 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
- customwas degassed under vacuum
- addition25% Aq. NH4OAc was then added
- extractionthe product was extracted in EtOAc
- dry with materialdried over Na2SO4
- custompurified by flash chromatography with EtOAc: toluene 2.5:97.5