HRID871818
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
- 110 °C
PROCEDURE
实验过程
Compound A (760 mg, 3.11 mmol), zinc (1.85 g, 28.2 mmol), and PdCl2(PPh3)2 (198 mg, 0.28 mmol) were charged in a two-necked bottle. The bottle was then vacuumed and purged with nitrogen, and dried toluene (30 mL), diethyl 4-iodobenzylphosphonate (0.65 mL, 2.82 mmol) or diethyl 3-iodobenzylphosphonate, and triethyl amine (3.91 mL, 28.2 mmol) were added to the bottle. The mixture in the bottle was heated to 110° C. for reaction for 48 hours, and the resulting was filtered to remove metal. The filtrate was condensed to remove the solvent, and then purified by column chromatography (ethyl acetate/hexanes=½) to obtain E (0.90 g, yield=70%) as white solid.
WORKUP
后处理
- additionwere added to the bottle
- filtrationthe resulting was filtered
- customto remove metal
- customcondensed
- customto remove the solvent
- custompurified by column chromatography (ethyl acetate/hexanes=½)
- customto obtain E (0.90 g, yield=70%) as white solid