反应详情

温度

62.5 °C

Piperidine (0.13 mL, 0.00132 mol) is added to a solution of 4-(3-bromopropyl)piperidine-1,4-dicarboxylic acid-1-tert-butyl ester-4-ethyl ester (0.1 gm, 0.00026 mol) in tetrahydrofuran (5 mL). The reaction mixture is heated at 60-65° C. for 3 hours. It is then cooled to room temperature, treated with demineralized water (12 mL) and extracted with ethyl acetate (2×20 mL). Combined extract is dried over sodium sulphate and concentrated under reduced pressure to get a crude residue which is purified by column chromatography (silica gel 230-400 mesh, methanol:dichloromethane, 1:9) to yield 4-(3-piperidin-1-yl propyl)piperidine-1,4-dicarboxylic acid-1-tert-butyl ester-4-ethyl ester.

1. temperatureIt is then cooled to room temperature
2. extractionextracted with ethyl acetate (2×20 mL)
3. extractionCombined extract
4. dry with materialis dried over sodium sulphate
5. concentrationconcentrated under reduced pressure
6. customto get a crude residue which
7. customis purified by column chromatography (silica gel 230-400 mesh, methanol:dichloromethane, 1:9)