関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Potassium Iodide | HCID 4875 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | Pyridine, 3-(2-chloroethyl)-, hydrochloride | HCID 199465 | — |
| 反応物 | N-[4-(piperidine-4-carbonyl)-phenyl]methanesulfonamide hydrochloride | HCID 14130042 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 4-(4-Methylsulfonylaminobenzoyl)-1-[2-(3-pyridyl)ethyl]piperidine dihydrochloride | HCID 14130046 | 28.8% |
反応手順
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/ispropanol to obtain 13.4 g of the intended compound.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05118689 |
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| 出典データセット | uspto-grants-1992_06 |
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| ORD ID | ord-8c78914681234ccf8397e0e2837f7883 |
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| 出典メモ | uspto-grants-1992_06 |
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