関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrogen Peroxide | HCID 784 | — |
| 反応物 | Acetonitrile | HCID 6342 | — |
| 反応物 | Cyclohexane | HCID 8078 | — |
| 反応物 | 1-Hydroxy-4-benzoyloxy-2,2,6,6-tetramethylpiperidine | HCID 688178 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 1-Cyclohexyloxy-4-benzoyloxy-2,2,6,6-tetramethylpiperidine | HCID 23372098 | 84% |
反応手順
A solution of 0.097 g (0.359 mmol) of ferric chloride hexahydrate 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, 28 ml of acetonitrile, and 19 ml of cyclohexane. The mixture is heated to 56° C. A solution of 4.70 g (69 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 mixture is heated at reflux for 45 minutes. Work-up and purification according to the procedure of Example 5 afford 5.47 g (84% yield) of the title compound, a pale yellow syrup. GC assay is 100%.
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-08c14529a5624a229bb297bff01f9af8 |
|---|
| 出典メモ | uspto-grants-2008_06 |
|---|