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Water → 4,4'-diamino-2,2'-biphenyldisulfonic Acid benzene-1,4-dicarbonyl Chloride

HRID 1278513
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HRID 1278513 반응식
O.C(=O)([O-])[O-].[Na+].[Na+].[NH2:8][C:9]1[CH:10]=[C:11]([S:26]([OH:29])(=[O:28])=[O:27])[C:12]([C:15]2[C:16]([S:22]([OH:25])(=[O:24])=[O:23])=[CH:17][C:18]([NH2:21])=[CH:19][CH:20]=2)=[CH:13][CH:14]=1.[C:30]([Cl:41])(=[O:40])[C:31]1[CH:39]=[CH:38][C:34]([C:35]([Cl:37])=[O:36])=[CH:33][CH:32]=1>C(Cl)(Cl)Cl.C1C(C(Cl)=O)=CC(C(Cl)=O)=CC=1C(Cl)=O.C(O)C>[NH2:8][C:9]1[CH:10]=[C:11]([S:26]([OH:29])(=[O:28])=[O:27])[C:12]([C:15]2[C:16]([S:22]([OH:25])(=[O:24])=[O:23])=[CH:17][C:18]([NH2:21])=[CH:19][CH:20]=2)=[CH:13][CH:14]=1.[C:34]1([C:35]([Cl:37])=[O:36])[CH:33]=[CH:32][C:31]([C:30]([Cl:41])=[O:40])=[CH:39][CH:38]=1
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참가 물질

8

반응물 4

HCID 962WaterHCID 7488Terephthaloyl chloride2회HCID 83372,2'-Benzidinedisulfonic acidHCID 10340Sodium Carbonate

생성물 1

HCID 867584924,4'-diamino-2,2'-biphenyldisulfonic Acid benzene-1,4-dicarbonyl Chloride수율 89.5%

시약·촉매·용매 3

HCID 78138
Trimesoyl chloride
촉매
HCID 702Ethanol용매
HCID 6212Chloroform용매4회

실험 절차

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.

후처리

  1. customInto a 1-L fluted round-bottom flask equipped with a mechanical stirring shaft
  2. dissolutionis dissolved
  3. customis obtained
  4. customis prepared
  5. customis also prepared
  6. stirringThe reaction flask is stirred at high speed (800-1000 rpm)
  7. stirringThe mixture is stirred for five minutes
  8. customresulting in an emulsion
  9. additionadded to the flask as quickly as possible
  10. stirringThe reaction mixture is stirred at high speed at room temperature for 2-3 hours
  11. additionAt the end of this period the thickened gel-like solution is poured into large flask
  12. filtrationThe resulting solid is filtered
  13. customdried in a vacuum oven

출처 및 근거

ORD 기록
ord-9b92e4f9c4f84fa29f7f3ffdb3c50d8f
출처 데이터셋
uspto-grants-2002_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06444091B1

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