反应详情

A solution of 22.4 g of 1-[2-(4-pyridinylamino)benzoyl]piperidine (Example 1b) in 45 ml of dimethylformamide was added dropwise to a suspension of sodium amide (from 4.8 g of 50% oil suspension, washed free of oil) in 115 ml of dimethylformamide. The mixture was stirred for one hour, and then 6.5 g of ethyl iodide was added dropwise. The reaction mixture was stirred for two hours, then filtered and concentrated in vacuo. The residue was partitioned between water and ether and the ether-soluble material recovered (15.2 g). The latter was recrystallized from ethyl acetate--pentane to give 13 g of 1-{2-[ethyl-(4-pyridinyl)amino]benzoyl}piperidine, m.p. 123°-124° C.

1. stirringThe reaction mixture was stirred for two hours
2. filtrationfiltered
3. concentrationconcentrated in vacuo
4. customThe residue was partitioned between water and ether
5. customthe ether-soluble material recovered (15.2 g)
6. customThe latter was recrystallized from ethyl acetate