HRID622118

反应详情

EQUATION

反应方程式

HRID 622118 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

1-Bromo-12-methyl-11-tridecene (4.4 g, 16 mmoles) and triphenylphosphine (4.65 g, 17 mmoles) dissolved in acetonitrile (80 ml) were heated to reflux for 4 days, cooled and concentrated in vacuo. The residue was chromatographed on silica gel eluted with chloroform and then with methanol-chloroform (2:3). Fractions containing the product were concentrated in vacuo, triturated with ether, filtered and dried in vacuo to afford the desired phosphonium salt.

WORKUP

后处理

  1. temperaturewere heated
  2. temperatureto reflux for 4 days
  3. temperaturecooled
  4. concentrationconcentrated in vacuo
  5. customThe residue was chromatographed on silica gel
  6. washeluted with chloroform
  7. additionFractions containing the product
  8. concentrationwere concentrated in vacuo
  9. customtriturated with ether
  10. filtrationfiltered
  11. customdried in vacuo