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1,1-Dimethoxycyclohexane → 1-Methoxy-1-[(2-methylbutan-2-yl)peroxy]cyclohexane
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 1,1-Dimethoxycyclohexane | HCID 13616 | — |
| 反応物 | tert-Amyl hydroperoxide | HCID 76962 | — |
| 触媒 | p-Toluenesulfonic acid | HCID 6101 | — |
| 溶媒 | Dimethyl Sulfoxide | HCID 679 | — |
| 生成物 | 1-Methoxy-1-[(2-methylbutan-2-yl)peroxy]cyclohexane | HCID 14573036 | 77.4% |
反応手順
A mixed solution consisting of 15.9 g of dimethyl sulfoxide and 1.2 g of p-toluenesulfonic acid was kept at 20° C., into which was added dropwise another solution consisting of 29.1 g of cyclohexanone-dimethylacetal and 21.1 g of 1,1-dimethylpropyl hydroperoxide. The resulting solution had an acid concentration of 0.1 mol/kg of the solution. The solution was treated in the same manner as described in Example 1 to obtain 33.8 g (yield: 67%) of crude 1-methoxy-1-(1,1-dimethylpropylperoxy)cyclohexane having a purity of 86%. The resulting crude peroxyketal was distilled at 43°-45° C. under a vacuum of 0.1 mmHg to obtain a purified peroxyketal having a purity of 98%.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05004780 |
| 出典データセット | uspto-grants-1991_04 |
| ORD ID | ord-894a0d2ba051497b83f47d4f19a68f62 |
| 出典メモ | uspto-grants-1991_04 |