関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Acetic Acid | HCID 176 | — |
| 反応物 | Oxygen | HCID 977 | — |
| 反応物 | 6'-Methyl-2'-acetonaphthone | HCID 598085 | — |
| 触媒 | Manganous Acetate | HCID 12525 | — |
| 触媒 | Hastelloy C | HCID 11332432 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 6-Methylnaphthalene-2-carboxylic acid | HCID 816843 | 69.6% |
反応手順
A Hastelloy C autoclave equipped with heater, stirrer, gas introduction tube, temperature sensor, pressure gauge and pressurized reflux condenser was charged with 100 g of 2-acetyl-6-methylnaphthalene, 380 g of acetic acid, 20 g of water and 15 g of manganese(II) acetate. Compressed air was passed, with stirring, through the solution at 140° C. and a pressure of 25 bar, with a gas escape rate of 3 liters per minute. The reaction was observed by continuously measuring the oxygen content in the exhaust gas. When this oxygen content returned to the initial level of 21% after a reaction time of 105 minutes, the air feed was shut off, the reaction mixture was cooled, with stirring, to room temperature, filtered, and the filter cake washed with 300 g of a 95 wt.-% solution of acetic acid. 70.3 g of 6-methyl-2-naphthoic acid (69.3% of the theory) was obtained, in a purity of 99.5%.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04764638 |
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| 出典データセット | uspto-grants-1988_08 |
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| ORD ID | ord-e23fbcdbda1948c7beb3352819fe23e4 |
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| 出典メモ | uspto-grants-1988_08 |
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