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Water → 3,3'-Diamino-4,4'-di-2-furoylaminobiphenyl

HRID 49749
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 49749
O.[N+:2]([C:5]1[CH:6]=[C:7]([C:19]2[CH:24]=[CH:23][C:22]([NH:25][C:26]([C:28]3[O:29][CH:30]=[CH:31][CH:32]=3)=[O:27])=[C:21]([N+:33]([O-])=O)[CH:20]=2)[CH:8]=[CH:9][C:10]=1[NH:11][C:12]([C:14]1[O:15][CH:16]=[CH:17][CH:18]=1)=[O:13])([O-])=O.[Cl-].[NH4+].[In]>C(O)C.CN1CCCC1=O>[NH2:33][C:21]1[CH:20]=[C:19]([C:7]2[CH:8]=[CH:9][C:10]([NH:11][C:12]([C:14]3[O:15][CH:16]=[CH:17][CH:18]=3)=[O:13])=[C:5]([NH2:2])[CH:6]=2)[CH:24]=[CH:23][C:22]=1[NH:25][C:26]([C:28]1[O:29][CH:30]=[CH:31][CH:32]=1)=[O:27]
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

7

Edukt 4

HCID 962WaterHCID 25517Ammonium ChlorideHCID 5359967IndiumHCID 227415993,3'-Dinitro-4,4'-di-2-furoylaminobiphenyl

Produkt 1

HCID 227416023,3'-Diamino-4,4'-di-2-furoylaminobiphenylAusbeute 23,3 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 702
Ethanol
Lösungsmittel
HCID 13387N-methyl-2-pyrrolidoneLösungsmittel

Reaktionsbedingungen

Temperatur
80 °C

Versuchsvorschrift

Into a separable flask equipped with a stirrer and a reflux condenser cooled with water, 7.4 g of 3,3′-dinitro-4,4′-di-2-furoylaminobiphenyl, 100 ml of N-methyl-2-pyrrolidone and 75 ml of ethyl alcohol were placed. After adding 40 ml of a saturated aqueous solution of ammonium chloride, 25.6 g of powder of indium metal was added to the prepared solution. The obtained mixture was stirred at 80° C. for 1 hour. After the reaction solution was cooled to the room temperature, the solid substance was removed by filtration. The filtrate was concentrated to about one half at a reduced pressure. To the concentrated filtrate, 300 ml of water was added and the formed solid substance was separated by filtration to obtain 2.9 g of a crude product. The crude product was purified in accordance with the silica gel column chromatography to obtain 1.5 g of 3,3′-diamino-4,4′-di-2-furoylaminobiphenyl. The yield of the isolated product was 23%. This product was recrystallized from N-methyl-2-pyrrolidone/ethyl acetate (the volume ratio: 25/75) and needle crystals having a decomposition temperature of 256 to 259° C. were obtained.

Aufarbeitung

  1. customInto a separable flask equipped with a stirrer and a reflux condenser
  2. additionwas added to the prepared solution
  3. temperatureAfter the reaction solution was cooled to the room temperature
  4. customthe solid substance was removed by filtration
  5. concentrationThe filtrate was concentrated to about one half at a reduced pressure
  6. additionTo the concentrated filtrate, 300 ml of water was added
  7. customthe formed solid substance was separated by filtration
  8. customto obtain 2.9 g of a crude product
  9. customThe crude product was purified in accordance with the silica gel column chromatography

Quellen und Nachweise

ORD-Eintrag
ord-70a34d2cf4ca4b2c893e159113b9d888
Quelldatensatz
uspto-grants-2004_03
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US06709804B2

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