Potassium Iodide → 4-Methylsulfonylaminobenzoyl-1-[3-(4-pyridyl)-propyl]piperidine dihydrochloride

온도

85 °C

0.295 g (0.926 mmol) of 4-(4-methylsulfonylaminobenzoyl)piperidine hydrochloride and 0.380 g (4.52 mmol) of sodium hydrogencarbonate were suspended in 4 ml of dimethylformamide and the suspension was stirred at 85° C. for 40 min. 0.20 g (1.04 mmol) of 4-(3-chloropropyl)pyridine hydrochloride and 0.31 g (1.87 mmol) of potassium iodide were added to the suspension and the mixture was stirred at 85° C. for 1.5 h. The liquid reaction mixture was filtered and the filtrate was concentrated. The obtained residue was purified according to silica gel column chromatography (chloroform:methanol:aqueous ammonia=96:4:0.4). The purified product was converted into its hydrochloride with ethanolic hydrogen chloride and recrystallized from ethanol to obtain 0.288 g (66%) of the intended compound.

1. stirringthe mixture was stirred at 85° C. for 1.5 h
2. customThe liquid reaction mixture
3. filtrationwas filtered
4. concentrationthe filtrate was concentrated
5. customThe obtained residue was purified
6. customrecrystallized from ethanol

ORD 기록

ord-d7b12f61fb6940d1bc62984f20a4cd13

출처 데이터셋

uspto-grants-1989_10

DOI

10.6084/m9.figshare.5104873.v1

특허 번호

US04876262