反应详情

A mixture of 4-[2,2-bis(3-methoxyphenyl)ethenyl]piperidine (1.65 g), 3-(8-chloroctyl)pyridine (1.13 g), sodium iodide (0.75 g) and anhydrous sodium carbonate (0.53 g) in dimethylformamide (10 ml) was stirred under argon at 75° for 16 hours. The solvent was removed in vacuo and the residue was taken up in a mixture of ethyl acetate and 1N sodium hydroxide solution. The separated aqueous layer was reextracted with three portions of ethyl acetate. The organic layers were washed in turn with water and brine, then were combined, dried over sodium sulfate, decolorized with charcoal and evaporated to give 2.5 g of crude product as an oil. The oil was purified by HPLC (hexane:ethyl acetate:triethylamine; 34:17:1) to give 1.8 g of 3-[8-[4-[2,2-bis(3-methoxyphenyl)ethenyl]-1-piperidinyl]octyl]pyridine, as an oil.

1. customThe solvent was removed in vacuo
2. additionthe residue was taken up in a mixture of ethyl acetate and 1N sodium hydroxide solution
3. washThe organic layers were washed in turn with water and brine
4. dry with materialdried over sodium sulfate
5. customevaporated
6. customto give 2.5 g of crude product as an oil
7. customThe oil was purified by HPLC (hexane:ethyl acetate:triethylamine; 34:17:1)