関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Acetone | HCID 180 | — |
| 反応物 | Sulfuric Acid | HCID 1118 | — |
| 反応物 | 1,1,3,3-Tetramethylbutyl hydroperoxide | HCID 79877 | — |
| 溶媒 | Pentane | HCID 8003 | — |
| 生成物 | 2,2-Di-(t-Octylperoxy) Propane | HCID 20196892 | 47.8% |
反応手順
To a jacketed reactor was charged 7.0g. (0.12 mole) of acetone, 39.2g. (0.24 mole) of 1,1,3,3-tetramethylbutyl hydroperoxide (89.7% assay) and 120 ml. of pentane. To the vigorously stirred solution at 0°C was added 16g. of 77% sulfuric acid over a period of 30 minutes and the reaction mixture was allowed to stir at 0°C for 4 hours. The pentane layer was then separated, washed with water, then aqueous 10% KOH solution and finally with water to neutral and was dried over anhyd. MgSO4. After separation of the desiccant and vacuum stripping, 21.3g. (53.1% of theory, uncorr.) of liquid remained which had an "active oxygen" content of 8.66% (theory, 9.64%). Hence, the assay was 90% and the corrected yield was 47.8%. An infrared spectrum of the product showed no O--H or C=O bands but showed a strong OO band at 860 cm-1.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US03950432 |
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| 出典データセット | uspto-grants-1976_04 |
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| ORD ID | ord-c0211e4f19ee41d59a436bc231c8a2a3 |
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| 出典メモ | uspto-grants-1976_04 |
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