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Dimethylamine → 2-(2'-Hydroxy-3'5-di-tert-butylphenyl) benzotriazole

HRID 1030311
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1030311
[OH:1][C:2]1[C:7]([C:8]([CH3:11])([CH3:10])[CH3:9])=[CH:6][C:5]([C:12]([CH3:15])([CH3:14])[CH3:13])=[CH:4][C:3]=1[N:16]1[N+:20]([O-])=[C:19]2[CH:22]=[CH:23][CH:24]=[CH:25][C:18]2=[N:17]1.C1(C)C=CC=CC=1.CNC.[H][H]>[C].[Pd].O>[OH:1][C:2]1[C:7]([C:8]([CH3:11])([CH3:10])[CH3:9])=[CH:6][C:5]([C:12]([CH3:13])([CH3:14])[CH3:15])=[CH:4][C:3]=1[N:16]1[N:20]=[C:19]2[CH:22]=[CH:23][CH:24]=[CH:25][C:18]2=[N:17]1
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

7

Edukt 4

HCID 674DimethylamineHCID 1140TolueneHCID 3413862,4-Di-tert-butyl-6-(1-oxo-2H-1lambda~5~,2,3-benzotriazol-2-yl)phenolHCID 178418361HCID 178418361, Verbindung3×

Produkt 1

HCID 774552-(2'-Hydroxy-3'5-di-tert-butylphenyl) benzotriazoleAusbeute 73,2 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 178418390HCID 178418390, VerbindungKatalysator
HCID 962WaterLösungsmittel

Reaktionsbedingungen

Temperatur
50 °C

Versuchsvorschrift

10 g (0.03 mol) of 2-(2'-hydroxy-3',5'-di-t-butylphenyl)benzotriazole-N-oxide, 100 mg of palladium carbon, 100 ml of a solvent mixture comprising toluene and water (ratio by volume, 4:1) and 3 g of 50% dimethylamine were charged into a 500-ml autoclave equipped with an agitator. After the air in the autoclave had been replaced by hydrogen, the pressure of hydrogen was set to 10 kg/cm2. The temperature was increased to 50° C. under agitation, and reaction was effected at the same temperature while agitation being continued until no more hydrogen was absorbed by the mixture. After the reaction had been completed, the autoclave was cooled, and the catalyst was filtered off. When part of the filtrate was subjected to quantitative analysis using GC, it was found that the yield of 2-(2'-hydroxy-3',5'-di-t-butylphenyl)benzotriazole is 85.6%. After the solvent had been distilled off from the filtrate, the residual solid was crystallized by ethanol and then washed with ethanol to obtain 7.1 g of 2-(2'-hydroxy-3',5'-di-t-butylphenyl)benzotriazole (yield, 71%; melting point, 152° to 155° C.).

Aufarbeitung

  1. additionwere charged into a 500-ml autoclave
  2. customequipped with an agitator
  3. customwas absorbed by the mixture
  4. temperaturethe autoclave was cooled
  5. filtrationthe catalyst was filtered off
  6. distillationAfter the solvent had been distilled off from the filtrate
  7. customthe residual solid was crystallized by ethanol
  8. washwashed with ethanol

Quellen und Nachweise

ORD-Eintrag
ord-4781fb17fbef4ba4a9a69b40ee13604c
Quelldatensatz
uspto-grants-1992_04
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US05104992

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