참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Hydrazine | HCID 9321 | — |
| 반응물 | Sodium Hydroxide | HCID 14798 | — |
| 반응물 | gamma-Oxo-4-(perylen-1-yl)butanoic acid | HCID 86645554 | — |
| 용매 | Diethylene Glycol | HCID 8117 | — |
| 생성물 | Perylenebutanoic acid | HCID 86605548 | 99.8% |
반응 단계
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.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08475685B2 |
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| 출처 데이터셋 | uspto-grants-2013_07 |
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| ORD ID | ord-d38c11e224bd41f6b9c6095757efb3f8 |
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| 출처 메모 | uspto-grants-2013_07 |
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