反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- customThe solvent was removed under reduced pressure
- customthe residue was triturated with 150 ml of ethyl ether
- filtrationthe precipitate was filtered off
- washThe ethereal solution was washed with 50 ml of H 0 and 50 ml of brine
- dry with materialdried over MgSO4
- customevaporated
- customto yield 2.96 g of crude title compound as a milky oil
- customPurification by flash chromatography on 300 g of Merck 9385 silica
- washeluted with 7:93 ethyl acetate