참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Toluene | HCID 1140 | — |
| 반응물 | Sodium Hydroxide | HCID 14798 | — |
| 반응물 | 4-Hydroxy-2,2,6,6-tetramethylpiperidine | HCID 75471 | — |
| 촉매 | Tetrabutylammonium Bromide | HCID 74236 | — |
| 용매 | Water | HCID 962 | — |
| 생성물 | 2,2,6,6-Tetramethyl-4-[(oxiran-2-yl)methoxy]piperidine | HCID 14274506 | — |
반응 단계
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%.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US05616637 |
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| 출처 데이터셋 | uspto-grants-1997_04 |
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| ORD ID | ord-a31b47d114774dcabb8fc53bf13ce8aa |
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| 출처 메모 | uspto-grants-1997_04 |
|---|