関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Methanesulfonic Acid | HCID 6395 | — |
| 反応物 | 3,5,5-TRIMETHYL-3-(t-BUTYLPEROXY)CYCLOHEXANONE | HCID 20570473 | — |
| 反応物 | HCID 178418361 | HCID 178418361 | — |
| 触媒 | Platinum | HCID 23939 | — |
| 溶媒 | Diethyl Ether | HCID 3283 | — |
| 生成物 | 3,5,5-Trimethyl-3-(t-butylperoxy) cyclohexanol | HCID 20306798 | — |
反応手順
The catalytic hydrogenation of 3,5,5-trimethyl-3-(t-butylperoxy)-cyclohexanone, 10.0 g. (0.045 mole), was carried out in a Parr Hydrogenation Apparatus using 1.0 g. 5% Platinum on carbon catalyst and in the presence of 50 ml. of 10% methanesulfonic acid solution. The hydrogenation at 60 p.s.i.g. hydrogen pressure was started at 0° C. and the temperature allowed to rise to 21° C. After 2 1/2 hours, the reaction was stopped, the product taken up in ether, the etheral solution washed to neutrality with water, dried over anhydrous magnesium sulfate and the ether removed under reduced pressure. Examination of the IR spectrum of the product showed that some of the desired product had been obtained as evidenced by the hydroxyl absorption band while some unreduced carbonyl was still present. Further catalytic hydrogenation at 35° C. for 18 hours caused a further increase in hydroxyl absorption band and reduction of the carbonyl absorption band.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04115455 |
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| 出典データセット | uspto-grants-1978_09 |
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| ORD ID | ord-36143b888cef4e3a95fe33787ddc8c89 |
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| 出典メモ | uspto-grants-1978_09 |
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