참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Water | HCID 962 | — |
| 반응물 | Terephthaloyl chloride | HCID 7488 | — |
| 반응물 | 2,2'-Benzidinedisulfonic acid | HCID 8337 | — |
| 반응물 | Sodium Carbonate | HCID 10340 | — |
| 촉매 | Trimesoyl chloride | HCID 78138 | — |
| 용매 | Ethanol | HCID 702 | — |
| 용매 | Chloroform | HCID 6212 | — |
| 생성물 | 4,4'-diamino-2,2'-biphenyldisulfonic Acid benzene-1,4-dicarbonyl Chloride | HCID 86758492 | 89.5% |
반응 단계
Into a 1-L fluted round-bottom flask equipped with a mechanical stirring shaft, is placed 250 mL of deionized water and 7.95 g of sodium carbonate. The mixture is stirred until the carbonate salt is dissolved. Then, 7.64 g of 4,4′-diamino-2,2′-biphenyldisulfonic acid (DABS, 85%) is added and stirring is continued until a homogeneous solution is obtained. A solution containing 2.00 g of PEG 400 distearate surfactant dissolved in 100 mL of purified chloroform is prepared and set aside. Another solution containing 3.79 g of terephthaloyl chloride and 0.05 g of 1,5-benzenetricarbonyl trichloride dissolved in 100 mL of purified chloroform is also prepared. The reaction flask is stirred at high speed (800-1000 rpm), and the chloroform/surfactant solution is added quickly to the flask. The mixture is stirred for five minutes, resulting in an emulsion. Then, the chloroform solution containing the terephthaloyl chloride added to the flask as quickly as possible. The reaction mixture is stirred at high speed at room temperature for 2-3 hours. At the end of this period the thickened gel-like solution is poured into large flask containing 300 mL ethanol/900 mL acetone. The resulting solid is filtered and dried in a vacuum oven to provide 9.15 grams of the desired polymer as a fluff, light purple solid.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US06444091B1 |
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| 출처 데이터셋 | uspto-grants-2002_09 |
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| ORD ID | ord-9b92e4f9c4f84fa29f7f3ffdb3c50d8f |
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| 출처 메모 | uspto-grants-2002_09 |
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