関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 1-(4-Pyridyl)piperazine | HCID 70517 | — |
| 反応物 | 4-fluoro-N-methylbenzene-1-sulfonamide | HCID 2440054 | — |
| 溶媒 | N-methyl-2-pyrrolidone | HCID 13387 | — |
| 生成物 | N-Methyl-4-[4-(4-pyridyl)piperazin-1-yl]benzenesulphonamide | HCID 21283536 | 6.9% |
反応手順
A mixture of 1-(4-pyridyl)piperazine (0.86 g), N-methyl-4-fluorobenzenesulphonamide (1.00 g) and potassium carbonate (2.00 g) in N-methylpyrrolidone was stirred at 100° C. for 24 hours and then evaporated. The residue was partitioned between dichloromethane and 2N hydrochloric acid. The acid layer was washed with dichloromethane, filtered and made basic with sodium bicarbonate solution. The mixture was extracted several times with chloroform, and the combined extracts were washed with water, dried over magnesium sulphate and evaporated. The residue was crystallised from ethanol/ethyl acetate to give the title compound (0.12 g), m.p. 204°-206° C. Found: C,57.55; H,6.13; N,16.62. C16H20N4O2S requires: C,57.81; H,6.06; N,16.85%.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04788196 |
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| 出典データセット | uspto-grants-1988_11 |
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| ORD ID | ord-542a1ec6e4ad4a5d9140fb585b095058 |
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| 出典メモ | uspto-grants-1988_11 |
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