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
[I; Ar is 3,4-methylenedioxyphenyl, R0 is H, R' is CH3CO, R" is CH3CH2CO, Y is C(C2H5)=CHCH2CH2 ] was prepared from 23.2 g. of 3-ethyl-6-(3,4-methylenedioxyphenyl)-3-hexenyl iodide (Preparation D1) and 22.3 g. of the lithium salt of 2,4-hexanedione (prepared by the procedure described in Example 8 below) in 300 ml. of dimethylformamide according to the procedure described above in Example 2. There was thus obtained 21 g. of crude product which was chromatographed on 600 g. of silica gel in pentane solution containing 20% benzene. The column was eluted with the pentane-benzene-ether solvent series. Benzene containing 3% ether brought out the desired product, 14.5 g. of 3-[3-ethyl-6-(3,4-methylenedioxyphenyl)-3-hexenyl]-2,4-hexanedione as a yellow oil.
WORKUP
后处理
- customwas prepared from 23.2 g
- customof crude product which was chromatographed on 600 g
- additionof silica gel in pentane solution containing 20% benzene
- washThe column was eluted with the pentane-benzene-ether solvent series