HRID249124

反应详情

EQUATION

反应方程式

HRID 249124 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 2.47 g of the above farnesyl bromide in 20 ml of dry dimethyformamide (DMF) at room temperature under argon was treated with 1.83 g (9.9 mmol, 1.1 eq.) of potassium phthalimide and stirred for 3 hours at room temperature. The solvent was removed under reduced pressure, the residue was triturated with 150 ml of ethyl ether, and the precipitate was filtered off. The ethereal solution was washed with 50 ml of H 0 and 50 ml of brine, dried over MgSO4 and evaporated to yield 2.96 g of crude title compound as a milky oil. Purification by flash chromatography on 300 g of Merck 9385 silica, eluted with 7:93 ethyl acetate:petroleum ether afforded 2.56 g (81%) of the desired product as a colorless oil.

WORKUP

后处理

  1. customThe solvent was removed under reduced pressure
  2. customthe residue was triturated with 150 ml of ethyl ether
  3. filtrationthe precipitate was filtered off
  4. washThe ethereal solution was washed with 50 ml of H 0 and 50 ml of brine
  5. dry with materialdried over MgSO4
  6. customevaporated
  7. customto yield 2.96 g of crude title compound as a milky oil
  8. customPurification by flash chromatography on 300 g of Merck 9385 silica
  9. washeluted with 7:93 ethyl acetate