참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Tetrachloro-p-hydroquinone | HCID 66603 | — |
| 반응물 | Tetrafluorophthalonitrile | HCID 74600 | — |
| 반응물 | Potassium Fluoride | HCID 522689 | — |
| 용매 | Acetonitrile | HCID 6342 | — |
| 생성물 | 1,4-Bis(3,4-dicyanotrifluorophenoxy)tetrachlorobenzene | HCID 11330937 | 84.4% |
반응 단계
In a 500 ml 4-necked flask, were poured 71.15 g (355 mmol) of tetrafluorophthalonitrile, 2.16 g (37.1 mmol) of potassium fluoride and 210 g of acetonitrile, and resulting was heated to 80° C. This mixture was kept at 80° C. with stirring, and to this mixture were dropped 4.40 g (17.7 mmol) of tetrachlorohydroquinone in 200 ml of acetonitrile over 1 hour. After dropping, reaction was performed at 80° C. for 6 hours. The reaction solution was cooled, filtrated, and the resulting residue washed with 30 ml and 15 ml of acetonitrile. After the filtrate had been concentrated on an evaporator to remove the solvent, 62.34 g of tetrafluorophthalonitrile was removed under in vacuo. To this was poured 27 ml of toluene and reflux performed for 1 hour. After cooling, the residue was washed with 5 ml, 25 ml and 5 ml of toluene, respectively, and further 12 ml of deionized water for three times. Finally, by drying the residue at 70° C. in vacuo, 9.08 g of 1,4-bis(3,4-dicyanotrifluorophenoxy)tetrachlorobenzene were obtained (yield: 84%).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US06916959B2 |
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| 출처 데이터셋 | uspto-grants-2005_07 |
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| ORD ID | ord-1221684185074235ab6ef124b2e9f4a4 |
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| 출처 메모 | uspto-grants-2005_07 |
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