関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrazine | HCID 9321 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | gamma-Oxo-4-(perylen-1-yl)butanoic acid | HCID 86645554 | — |
| 溶媒 | Diethylene Glycol | HCID 8117 | — |
| 生成物 | Perylenebutanoic acid | HCID 86605548 | 99.8% |
反応手順
The compound 72 (0.390 g, 1.11 mmol), 0.4 ml of 79% aqueous hydrazine, and 0.290 g (7.25 mmol) of sodium hydroxide were dissolved in 3.0 ml of diethylene glycol, followed by 90-minute refluxing in a 180-° C. oil bath. The excess hydrazine and water were distilled away, and the refluxing was continued for two more hours. After the reaction was completed, the solution was cooled back to room temperature, to precipitate a solid substance. The solid substance was collected by filtration, and was washed with ion-exchange water and 2M hydrochloric acid, followed by drying under reduced pressure. This solid substance was dispersed in 10 ml of xylene, and was heated to 140° C. In this manner, the solid substance was dissolved. After that, the substance was cooled slowly back to room temperature, to precipitate a solid substance. The solid substance generated here was collected by filtration, and was dried under reduced pressure, to obtain 0.375 g of the black solid substance 73.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08475685B2 |
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| 出典データセット | uspto-grants-2013_07 |
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| ORD ID | ord-d38c11e224bd41f6b9c6095757efb3f8 |
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| 出典メモ | uspto-grants-2013_07 |
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