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2,2-Bis(3-nitro-4-hydroxyphenyl)hexafluoropropane → 2,2-Bis(3-amino-4-hydroxyphenyl)hexafluoropropane

HRID 1601749
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1601749
[N+:1]([C:4]1[CH:5]=[C:6]([C:11]([C:20]2[CH:25]=[CH:24][C:23]([OH:26])=[C:22]([N+:27]([O-])=O)[CH:21]=2)([C:16]([F:19])([F:18])[F:17])[C:12]([F:15])([F:14])[F:13])[CH:7]=[CH:8][C:9]=1[OH:10])([O-])=O>CO>[NH2:27][C:22]1[CH:21]=[C:20]([C:11]([C:6]2[CH:7]=[CH:8][C:9]([OH:10])=[C:4]([NH2:1])[CH:5]=2)([C:12]([F:13])([F:14])[F:15])[C:16]([F:17])([F:18])[F:19])[CH:25]=[CH:24][C:23]=1[OH:26]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

3

Edukt 1

HCID 111336832,2-Bis(3-nitro-4-hydroxyphenyl)hexafluoropropane

Produkt 1

HCID 6326032,2-Bis(3-amino-4-hydroxyphenyl)hexafluoropropane

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel

Versuchsvorschrift

400.0 g of 2,2-bis(3-nitro-4-hydroxyphenyl)hexafluoropropane and 1200 cc of methanol were put into a 2000-cc four-neck flask equipped with a thermometer, a Dimroth condenser and a stirrer, and stirred therein, to which was added 9.0 g (dry weight) of E196R/W5%Pd. This was heated and kept at 60 to 65° C. with stirring, to which was dropwise added 313.2 g of an aqueous solution of 60% hydrazine monohydrate over a period of 4 hours. After the aqueous hydrazine solution was added, the mixture was stirred for further 30 minutes, and then gradually cooled to room temperature. After the catalyst was removed through filtration, the reaction mixture was concentrated to obtain a crude product of 2,2-bis(3-amino-4-hydroxyphenyl)hexafluoropropane. The crude yield was 336.8 g (98%). The purity in liquid chromatography was 97.9% (area %).

Aufarbeitung

  1. customequipped with a thermometer
  2. additionto which was added
  3. dry with material9.0 g (dry weight) of E196R/W5%Pd
  4. temperatureThis was heated
  5. customkept at 60 to 65° C.
  6. stirringwith stirring, to which
  7. customof 4 hours
  8. additionAfter the aqueous hydrazine solution was added
  9. stirringthe mixture was stirred for further 30 minutes
  10. customAfter the catalyst was removed through filtration
  11. concentrationthe reaction mixture was concentrated

Quellen und Nachweise

ORD-Eintrag
ord-c06eb6fc8bd74f6a804d34be9daa10eb
Quelldatensatz
uspto-grants-1999_11
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US05977413

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