関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Toluene | HCID 1140 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | 4-Hydroxy-2,2,6,6-tetramethylpiperidine | HCID 75471 | — |
| 触媒 | Tetrabutylammonium Bromide | HCID 74236 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 2,2,6,6-Tetramethyl-4-[(oxiran-2-yl)methoxy]piperidine | HCID 14274506 | — |
反応手順
64.0 g of sodium hydroxide (1.6 mol) are dissolved in 64 ml of water under argon in a 750 ml sulfonation flask fitted with mechanical stirrer, condenser, thermometer and 100 ml dropping funnel. 170 ml of toluene, 10.3 g (31.8 mmol) of tetrabutylammonium bromide and 50 g (318 mmol) of 4-hydroxy-2,2,6,6-tetramethylpiperidine are added. 58.8 g (636 mmol) of epichlorohyrdin are added dropwise at 45° C. The mixture is then stirred at 50° C. for 4 hours. The reaction mixture is cooled to room temperature and poured into 1 l of ice water, and the organic phase is separated off, dried using sodium sulfate and evaporated on a rotary evaporator. The residue is distilled at 8×10-3 mmHg. Boiling point: 48° C., yield: 28 g (41%). GC: 98%.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05616637 |
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| 出典データセット | uspto-grants-1997_04 |
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| ORD ID | ord-a31b47d114774dcabb8fc53bf13ce8aa |
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| 出典メモ | uspto-grants-1997_04 |
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