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Aniline → HCID 10948950, Verbindung

HRID 1069810
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1069810
[OH:1][C:2]1[C:11]([C:12]([OH:14])=O)=[CH:10][C:9]2[C:4](=[CH:5][CH:6]=[C:7]([C:15]([OH:17])=O)[CH:8]=2)[CH:3]=1.[NH2:18][C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1.P(Cl)(Cl)Cl.C(=O)([O-])[O-].[Na+].[Na+]>C1(C)C(C)=CC=CC=1.O>[OH:1][C:2]1[C:11]([C:12]([NH:18][C:19]2[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=2)=[O:14])=[CH:10][C:9]2[C:4](=[CH:5][CH:6]=[C:7]([C:15]([NH:18][C:19]3[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=3)=[O:17])[CH:8]=2)[CH:3]=1
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

7

Edukt 4

HCID 6115AnilineHCID 10340Sodium CarbonateHCID 24387Phosphorus trichlorideHCID 98160552-Hydroxynaphthalen-3,6-dicarboxylic acid

Produkt 1

HCID 10948950HCID 10948950, VerbindungAusbeute 45,8 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 962
Water
Lösungsmittel
HCID 7237O-XyleneLösungsmittel

Reaktionsbedingungen

Temperatur
90 °C

Versuchsvorschrift

2-Hydroxy-3,6-dihydroxycarbonylnaphthalene (4.64 g) and aniline (4.10 g) were dispersed in xylene (92.8 g), followed by heating to 90° C. Phosphorous trichloride (2.4 g) was added dropwise at 90 to 100° C., and then the mixture was reacted at 140° C. for 3 hours. After the completion of the reaction, water (92.8 g) was added and the reaction solution was neutralized with sodium carbonate at 90° C. The solution was filtered at room temperature and washed in turn with xylene (46.4 g) and water (46.4 g). The resultant crystal was subjected to reflux washing using acetone (80 g) and then filtered. This operation was repeated three times, followed by drying to obtain 3.5 g of 2-hydroxy-3,6-diphenylaminocarbonylnaphthalene as a white powdered crystal (melting point: 314-317° C.).

Aufarbeitung

  1. customthe mixture was reacted at 140° C. for 3 hours
  2. additionwas added
  3. filtrationThe solution was filtered at room temperature
  4. washwashed in turn with xylene (46.4 g) and water (46.4 g)
  5. temperatureto reflux
  6. washwashing
  7. filtrationfiltered
  8. customby drying

Quellen und Nachweise

ORD-Eintrag
ord-0a07a9482a8846e0a1f9cb90a2e248cb
Quelldatensatz
uspto-grants-2001_06
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US06252104B1

Notizen zur Reaktion

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