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Phosphorus trichloride → HCID 20082255, Verbindung

HRID 1609784
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1609784
[C:1]([C:5]1[CH:10]=[C:9]([C:11]([CH3:14])([CH3:13])[CH3:12])[CH:8]=[C:7]([CH3:15])[C:6]=1[OH:16])([CH3:4])([CH3:3])[CH3:2].[P:17]([Cl:20])(Cl)Cl>CN(C)C=O.C1(C)C(C)=CC=CC=1>[C:1]([C:5]1[CH:10]=[C:9]([C:11]([CH3:14])([CH3:13])[CH3:12])[CH:8]=[C:7]([CH3:15])[C:6]=1[O:16][P:17]([Cl:20])[O:16][C:6]1[C:7]([CH3:15])=[CH:8][C:9]([C:11]([CH3:13])([CH3:12])[CH3:14])=[CH:10][C:5]=1[C:1]([CH3:4])([CH3:3])[CH3:2])([CH3:4])([CH3:3])[CH3:2]
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 2

HCID 24387Phosphorus trichlorideHCID 692244,6-Di-tert-butyl-o-cresol

Produkt 1

HCID 20082255HCID 20082255, VerbindungAusbeute 95 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 6228DimethylformamideKatalysatorHCID 7237O-XyleneLösungsmittel

Reaktionsbedingungen

Temperatur
50 °C

Versuchsvorschrift

890.3 g (4 mol) of 2,4-di-tert-butyl-6-methylphenol, 4.2 g of dimethylformamide and 170.0 g of xylene are introduced into a four-neck flask which has been flushed with nitrogen and is fitted with a thermometer, dropping funnel, reflux condenser and distillation attachment. 274.9 g (2 mol) of phosphorus trichloride are added dropwise with stirring over the course of 1.5 hours at a temperature of 50° C. The reaction mixture is warmed to 130° C. and refluxed at this temperature for 1 hour. The reaction mixture is kept at 120° C. for 1 hour under a vacuum of 0.15 bar. Xylene is subsequently removed by distillation under a greater vacuum. After the vacuum has been broken using nitrogen, 959.5 g (1.9 mol) of the title compound are obtained as supercooled, yellow-orange, clear melt.

Aufarbeitung

  1. customhas been flushed with nitrogen
  2. customis fitted with a thermometer
  3. temperaturereflux condenser
  4. distillationdistillation attachment
  5. temperatureThe reaction mixture is warmed to 130° C.
  6. temperaturerefluxed at this temperature for 1 hour
  7. waitThe reaction mixture is kept at 120° C. for 1 hour under a vacuum of 0.15 bar
  8. customXylene is subsequently removed by distillation under a greater vacuum

Quellen und Nachweise

ORD-Eintrag
ord-fe8bb390e62742689ba7acf0a2fca8fd
Quelldatensatz
uspto-grants-1995_03
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US05401845

Notizen zur Reaktion

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