反应详情

1.13 g (18.8 mmol) of sodium methoxide was added to a suspension of 3.0 g (9.4 mmol of 4-(4-methylsulfonylaminobenzoyl)piperidine hydrochloride and 1.55 g (9.4 mmol) of 4-chloromethyl-pyridine hydrochloride in 90 ml of acetonitrile. The mixture was stirred at room temperature for 10 min. 2.88 g of potassium carbonate was added to the mixture and the obtained mixture was refluxed for 3 h. After cooling, the liquid reaction mixture was filtered and the filtrate was concentrated, while the residue was purified according to silica gel chromatography (chloroform:methanol=95.5). The product was converted into its hydrochloride with ethanolic hydrogen chloride and recrystallized from methanol/isopropanol to obtain 1.4 g of the intended compound:

1. temperaturethe obtained mixture was refluxed for 3 h
2. temperatureAfter cooling
3. customthe liquid reaction mixture
4. filtrationwas filtered
5. concentrationthe filtrate was concentrated, while the residue
6. customwas purified
7. customrecrystallized from methanol/isopropanol