HRID2063936

反应详情

EQUATION

反应方程式

HRID 2063936 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 5-phenyl-pentane-1-ol (1.0 gm, 6.09 mmol) in CH2Cl2 (20 ml), triphenyl phosphine (2.35 gm, 8.52 mmol), imidazole (0.58 gm, 8.52 mmol) and elemental iodine (2.16 gm, 8.52 mmol) was stirred at room temperature for 12 h. The solvent was evaporated under reduced pressure. The residue was diluted with EtOAc (30 ml), H2O (20 ml) was added, separated and the organic phase was washed with brine (30 ml). The organic layer was dried over anhydrous Na2SO4; solvent was evaporated under reduced pressure and the crude product was purified by column chromatography using hexane as eluent. The crude product was purified by column chromatography using hexane as eluent. The pure product was an oily liquid (750 mg).

WORKUP

后处理

  1. customThe solvent was evaporated under reduced pressure
  2. additionThe residue was diluted with EtOAc (30 ml), H2O (20 ml)
  3. additionwas added
  4. customseparated
  5. washthe organic phase was washed with brine (30 ml)
  6. dry with materialThe organic layer was dried over anhydrous Na2SO4
  7. customsolvent was evaporated under reduced pressure
  8. customthe crude product was purified by column chromatography
  9. customThe crude product was purified by column chromatography