関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Potassium Iodide | HCID 4875 | — |
| 反応物 | Cyclohexanol | HCID 7966 | — |
| 反応物 | Sodium Carbonate | HCID 10340 | — |
| 反応物 | N,N-bis(2-chloroethyl)-p-toluenesulphonamide | HCID 96039 | — |
| 反応物 | 4-Methoxy-3,5-dimethylaniline HCl | HCID 19032380 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 4-(4-Methoxy-3,5-dimethylphenyl)-1-[(4-methylphenyl)sulfonyl]piperazine | HCID 19032387 | 50.4% |
反応手順
A mixture of 10 g of 4-methoxy-3,5-dimethylbenzenamine hydrochloride, 19.9 g of N,N-bis(2-chloroethyl)-4-methylbenzenesulfonamide, 16.8 g of sodium carbonate, 0.5 g of potassium iodide and 100 ml of cyclohexanol was stirred overnight at 150°-160° C. After cooling, the reaction mixture was poured into water. The product was extracted with dichloromethane. The extract was washed with water, dried, filtered and evaporated. The residue was purified by column-chromatography over silica gel using trichloromethane as eluent. The pure fractions were collected and the solvent was evaporated. The residue was crystallized from 1-butanol, yielding 10 g (50.4%) of 4-(4-methoxy-3,5-dimethylphenyl)-1-[(4-methylphenyl)sulfonyl]piperazine; mp. 174.2° C. (interm. 42).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05650411 |
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| 出典データセット | uspto-grants-1997_07 |
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| ORD ID | ord-defd8b78b9dd4aa5ae0b400304ec643c |
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| 出典メモ | uspto-grants-1997_07 |
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