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Mesityl oxide → HCID 20570470, Verbindung

HRID 1577965
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1577965
[O:1]=[C:2]([CH:4]=[C:5]([CH3:7])[CH3:6])[CH3:3].[C:8]([O:12][O:13][C:14]([CH3:23])([CH3:22])[CH2:15][CH2:16][C:17]([O:20][OH:21])([CH3:19])[CH3:18])([CH3:11])([CH3:10])[CH3:9]>>[CH3:6][C:5]([O:21][O:20][C:17]([CH3:19])([CH3:18])[CH2:16][CH2:15][C:14]([O:13][O:12][C:8]([CH3:11])([CH3:10])[CH3:9])([CH3:23])[CH3:22])([CH2:4][C:2](=[O:1])[CH3:3])[CH3:7]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

3

Edukt 2

HCID 8858Mesityl oxideHCID 1410462,5-Dimethyl-2-hydroperoxide-5-tert-butylperoxyhexane

Produkt 1

HCID 20570470HCID 20570470, VerbindungAusbeute 84,4 %

Versuchsvorschrift

A mixture of 19.62 g. (0.20 mole) of mesityl oxide, 61.40 g. (0.22 mole) of 4-t-butylperoxy-1,1,4,4-tetramethylbutyl hydroperoxide (84%) and 10.0 g. of Amberlyst 15® sulfonic acid type ion exchange resin was stirred for 16 hours at 28°-30° C. and then at 35° C. for 4 hours. The resin was separated by filtration and the filtrate subjected to steam distillation at 20 torr in the presence of sodium bicarbonate to maintain a slightly alkaline pH during the distillation. The distillation was ended when the removal of unreacted mesityl oxide was complete. The product was taken up in ether, the ether solution dried over anhydrous magnesium sulfate and the ether removed under reduced pressure. The product weighed 55.9 g. and was obtained in 84.4% yield.

Aufarbeitung

  1. additionA mixture of 19.62 g
  2. customThe resin was separated by filtration
  3. distillationthe filtrate subjected to steam distillation at 20 torr in the presence of sodium bicarbonate
  4. temperatureto maintain a slightly alkaline pH
  5. distillationduring the distillation
  6. distillationThe distillation
  7. customthe removal of unreacted mesityl oxide
  8. dry with materialthe ether solution dried over anhydrous magnesium sulfate
  9. customthe ether removed under reduced pressure
  10. customand was obtained in 84.4% yield

Quellen und Nachweise

ORD-Eintrag
ord-3eb57120c65343c684ca9f074e534b52
Quelldatensatz
uspto-grants-1981_09
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US04289914

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