関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Nitric Acid | HCID 944 | — |
| 反応物 | Toluene | HCID 1140 | — |
| 反応物 | Cyclohexanecarboxaldehyde, 2,2,6-trimethyl- | HCID 103695 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 2,2,6-Trimethylcyclohexanecarboxylic acid | HCID 14228714 | 98.9% |
反応手順
In a 300-ml 4-necked flask equipped with a condenser, a thermometer, a dropping funnel, and a stirrer was placed 39 g of nitric acid (60% aqueous solution) and heated to 55° C. To the solution was added dropwise 93 g (0.60 mole) of 2,2,6-trimethylcyclohexanecarbaldehyde (4) composed of 35% of the trans-form and 65% of the cis-form synthesized in Synthesis Example 1-A) described above over a period of 2 hours. Thereafter, the reaction was carried out for 3 hours at the same temperature. Then, 100 g of toluene and 100 g of water were added to the reaction mixture at room temperature to wash with water and form an organic layer and an aqueous layer separately. The organic layer was washed thrice with 100 g of a saturated aqueous sodium chloride solution, and the toluene was distilled off under reduced pressure by means of an evaporator, to provide 101 g of crude 2,2,6-trimethylcyclohexanecarboxylic acid (5) composed of 35% of the trans-form and 65% of the cis-form.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05288702 |
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| 出典データセット | uspto-grants-1994_02 |
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| ORD ID | ord-4a13ad68d4e24154b38053f6a3620f38 |
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| 出典メモ | uspto-grants-1994_02 |
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