関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Acetic Acid | HCID 176 | — |
| 反応物 | Hydrogen Peroxide | HCID 784 | — |
| 反応物 | Methanol | HCID 887 | — |
| 反応物 | Water | HCID 962 | — |
| 反応物 | 1-Hydroxy-4-benzoyloxy-2,2,6,6-tetramethylpiperidine | HCID 688178 | — |
| 溶媒 | Cyclohexane | HCID 8078 | — |
| 生成物 | 1-Cyclohexyloxy-4-benzoyloxy-2,2,6,6-tetramethylpiperidine | HCID 23372098 | 40% |
反応手順
A solution of 0.101 g (0.37 mmol) of ferric chloride hexahydrate and 0.115 g (1.9 mmol) of glacial acetic acid in 2 ml of water is added to a mixture of 5.00 g (18.1 mmol) of 1-oxyl-4-benzoyloxy-2,2,6,6-tetramethylpiperidine, 27 ml of methanol, and 18 ml of cyclohexane. The mixture is heated to reflux, 55° C. A solution of 4.9 g (72 mmol) of 50% aqueous hydrogen peroxide is added dropwise over 2.25 hours to the reaction mixture while the temperature is brought to and maintained at reflux. After the peroxide is added, the reaction mixture tests negative for hydrogen peroxide. The yield of the title compound, after work-up with ethyl acetate and purification by flash chromatography, is 2.63 g (40% yield, GC assay 100%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07390904B2 |
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| 出典データセット | uspto-grants-2008_06 |
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| ORD ID | ord-d30f20b90bff4edb90586a46d73f3455 |
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| 出典メモ | uspto-grants-2008_06 |
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