HRID1584782

反应详情

EQUATION

反应方程式

HRID 1584782 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of tributyl-(7-[1,3]dioxan-2-ylbenzofuran-5-yl)stannane (839 mg), 5-bromo-1-methyl-1H-[1,2,4]triazole (396 mg), bis(triphenylphosphine)palladium (II) chloride (59 mg) in dry toluene (10 ml) was heated at reflux for 42 h. The cooled solution was then filtered through Hyflo and the filtrate washed with 10% potassium fluoride solution (30 ml). The organic layer was washed with brine (30 ml), dried, and evaporated in vacuo to give a yellow oil. The crude material was purified by FCC eluting with hexane:ethyl acetate (1:1→1:3) to give the title compound as a yellow oil (171 mg,).

WORKUP

后处理

  1. temperaturewas heated
  2. temperatureat reflux for 42 h
  3. filtrationThe cooled solution was then filtered through Hyflo
  4. washthe filtrate washed with 10% potassium fluoride solution (30 ml)
  5. washThe organic layer was washed with brine (30 ml)
  6. customdried
  7. customevaporated in vacuo
  8. customto give a yellow oil
  9. customThe crude material was purified by FCC
  10. washeluting with hexane:ethyl acetate (1:1→1:3)