HRID871818

反应详情

EQUATION

反应方程式

HRID 871818 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

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

  1. additionwere added to the bottle
  2. filtrationthe resulting was filtered
  3. customto remove metal
  4. customcondensed
  5. customto remove the solvent
  6. custompurified by column chromatography (ethyl acetate/hexanes=½)
  7. customto obtain E (0.90 g, yield=70%) as white solid