反应详情

温度

40 °C

35 g (0.101 mol) of 4-(4-methylsulfonylaminobenzoyl)piperidine hydrochloride and 55 g of potassium carbonate were suspended in 700 ml of dimethylformamide and the suspension was stirred at 40° C. for 20 min. 19.6 g (0.101 mol) of 3-(2-chloroethyl)pyridine hydrochloride and 6.0 g (0.036 mol) of potassium iodide were added to the suspension and the mixture was stirred at 90° C. for 3.5 h. The liquid reaction mixture was filtered and the filtrate was concentrated, while the residue was purified according to silica gel chromatography (chloroform:methanol=93:7). The purified product was converted into its hydrochloride with ethanolic hydrogen chloride and recrystallized from methanol/isopropanol to obtain 13.4 g of the intended compound.

1. stirringthe mixture was stirred at 90° C. for 3.5 h
2. customThe liquid reaction mixture
3. filtrationwas filtered
4. concentrationthe filtrate was concentrated, while the residue
5. customwas purified
6. customrecrystallized from methanol/isopropanol