참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Sodium Chloride | HCID 5234 | — |
| 반응물 | tert-Butyl hydroperoxide | HCID 6410 | — |
| 반응물 | Bis(2,2,6,6-tetramethyl-4-piperidyl) succinate | HCID 93340 | — |
| 촉매 | Molybdenum oxide | HCID 139765 | — |
| 용매 | Cyclohexane | HCID 8078 | — |
| 생성물 | Bis(1-cyclohexyloxy-2,2,6,6-tetramethylpiperidin-4-yl) succinate | HCID 21026400 | 137.6% |
반응 단계
A two-phase mixture of 70% aqueous t-butyl hydroperoxide (103.9 g, 807 mmol), cyclohexane (200 ml) and sodium chloride (15 g) is shaken in a separatory funnel. The organic phase is dried over magnesium sulfate, filtered, and added to 40.0 g (101 mmol) of di-(2,2,6,6-tetramethylpiperidin-4-yl) succinate. Molybdenum oxide (2.0 g) is added, and the mixture is refluxed for one hour. Water is collected in a Dean-Stark trap. The entire reaction mixture is then transferred to a Fischer-Porter bottle and heated at 140° C. for 6 hours. Additional t-butyl hydroperoxide (90%, 10.1 g, 101 mmol) is added and heating is resumed for another 4 hours. The colorless reaction mixture is filtered, concentrated, and dissolved in heptane (20 0 ml). The heptane solution is passed through a short column of silica gel with heptane. Subsequent evaporation affords an oil which is crystallized from ethanol to yield 41.2 g (69%) of a white powder, m.p. 122°-6° C.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US05204473 |
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| 출처 데이터셋 | uspto-grants-1993_04 |
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| ORD ID | ord-a1480b7fb3654dbca29483403b9b58c6 |
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| 출처 메모 | uspto-grants-1993_04 |
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