関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Phenol | HCID 996 | — |
| 反応物 | 2-Isopropylphenol | HCID 6943 | — |
| 触媒 | Phosphoric acid, calcium nickel salt (1:?:?) | HCID 22174092 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 4-Isopropylphenol | HCID 7465 | — |
| 生成物 | p-Isopropenylphenol | HCID 584247 | — |
反応手順
A quartz tube 40 cm×16 mm, inside diameter, with Vigreux indentations 1" above the top of the bottom joint was packed with 3 cm of quartz rings, 28 cm (equivalent to 44.16 grams) of the calcium-nickel phosphate catalyst of formula I, which had previously been calcined at about 800° for a period of about 17 hours and then filled with additional quartz rings (for heat transfer). Thermocouples were placed on the side of the tube and the tube placed in a vertical furnace. At the top of the tube was placed a manifold from which the air and liquid feeds were added. At the bottom of the tube were placed in series three three-necked flasks, the first two being immersed in ice/water baths. The catalyst bed was heated to a temperature between 300°-500° with an air flow of 0.15 ft3 /hr. Then the liquid feed composed of phenol, water, and isopropylphenol in the molar ratio of 2.8:2.0:1.0 was introduced to provide an addition rate of 0.15 ml/min. After specified volumes of feed had been introduced, the products (phenol, water, the propylphenol and propenylphenol) were collected from the receiver and analyzed for para-isopropenylphenol content by NHMR spectroscopy (proton nuclear magnetic resonance). Table I shows the results of para-isopropenylphenol formation as a function of the moles of para-isopropylphenol used.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04346249 |
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| 出典データセット | uspto-grants-1982_08 |
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| ORD ID | ord-198fddb556a14b19994b429f4aa81760 |
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| 出典メモ | uspto-grants-1982_08 |
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