化工社化工社 化学情報印刷レポート · 研究参考用
Hydrogen Peroxide → N-cyclohexyloxy-4-oxo-2,2,6,6-tetramethylpiperidine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrogen Peroxide | HCID 784 | — |
| 反応物 | Methanesulfonic Acid | HCID 6395 | — |
| 反応物 | Cyclohexane | HCID 8078 | — |
| 反応物 | 1-Hydroxy-2,2,6,6-tetramethyl-4-oxopiperidine | HCID 98642 | — |
| 触媒 | Ferrous sulfate heptahydrate | HCID 62662 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | N-cyclohexyloxy-4-oxo-2,2,6,6-tetramethylpiperidine | HCID 22019868 | 35% |
反応手順
A solution of 20.1 g (0.295 mol) of 50% aqueous hydrogen peroxide is added over 6 hours at 60° C. to a mixture of 8.51 g (50.0 mmol) of 1-oxyl-2,2,6,6-tetramethylpiperid-4-one, 0.70 g (2.5 mmol) of iron(II) sulfate heptahydrate, 0.3 ml (5 mmol) of methanesulfonic acid, 11 ml of cyclohexane, and 90 ml of methanol. Shortly after the addition is completed, the reaction mixture tests negative for hydrogen peroxide. The reaction mixture is concentrated to afford 4.4 g (35% yield) of the title compound, isolated as a yellow oil. Structure is confirmed by mass spectrometry and NMR analysis.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07390904B2 |
| 出典データセット | uspto-grants-2008_06 |
| ORD ID | ord-a53408cb0ce54faa8f117c9a7ef781f0 |
| 出典メモ | uspto-grants-2008_06 |