関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Methanol | HCID 887 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | HCID 15289526 | HCID 15289526 | — |
| 反応物 | 1-Bromo-12-(4-phenylpiperazinyl)dodecane | HCID 19937754 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | N-(2,6-Diisopropylphenyl)-2-[12-(4-phenylpiperazinyl)dodecylthio]acetamide | HCID 19937767 | 57.2% |
反応手順
To a mixture of 1.47 g of N-(2,6-diisopropylphenyl)-2-(acetylthio)acetamide and 12 ml of methanol was added dropwise 1.7 ml of a 30% aqueous sodium hydroxide solution at 0° C. in an argon atmosphere. After stirring for 30 minutes, a mixture of 2.05 g of 1-bromo-12-(4-phenylpiperazinyl)dodecane synthesized in (1) above and 14 ml of methanol was added thereto, followed by stirring at 60° C. for 1 hour and then at room temperature for 16 hours. To the reaction mixture was added 100 ml of ethyl acetate, and the mixture was washed successively with water and a saturated sodium chloride aqueous solution, and dried over magnesium sulfate. The solvent was evaporated under reduced pressure, and the residue was subjected to column chromatography using a 1:2 mixture of ethyl acetate and hexane as a developing solvent. The resulting crystals were recrystallized from isopropyl alcohol-water to yield 1.66 g of the title compound as white powder (m.p.=76.5° -77.5° C.).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05416212 |
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| 出典データセット | uspto-grants-1995_05 |
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| ORD ID | ord-84b459ec96ee44ad9b0841d016b96fa3 |
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| 出典メモ | uspto-grants-1995_05 |
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