Triethylamine → HCID 20426788, Verbindung

HRID 434397

Reaktionsgleichung

Reaktionsgleichung von HRID 434397
[CH3:1][Si:2]([CH3:11])([CH3:10])[C:3]1[CH:8]=[CH:7][C:6]([OH:9])=[CH:5][CH:4]=1.C(N(CC)CC)C.[C:19](Cl)(=[O:22])[CH:20]=[CH2:21]>C1(C)C=CC=CC=1.C1(C=CC(O)=CC=1)O>[C:19]([O:9][C:6]1[CH:7]=[CH:8][C:3]([Si:2]([CH3:11])([CH3:10])[CH3:1])=[CH:4][CH:5]=1)(=[O:22])[CH:20]=[CH2:21]

Komponenten

6

Edukt 3

HCID 8471TriethylamineHCID 13140Acryloyl chlorideHCID 257324-(Trimethylsilyl)phenol

Produkt 1

HCID 20426788HCID 20426788, VerbindungAusbeute 83,5 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 785HydroquinoneKatalysatorHCID 1140TolueneLösungsmittel

Versuchsvorschrift

8.32 g (0.05 mole) of p-trimethylsilylphenol was dissolved in 25 ml toluene. 6.1 g (0.06 mole) triethyl amine and 0.05 g hydroquinone was added. The solution was warmed. 5.43 g (0.06 mole) of acryloyl chloride was added over a 15 minute period. After 11/2 hours, the solution was washed two times with 5 percent sodium carbonate in water and separated. After washing with brine and separating, the organic phase was dried over magnesium sulfate, filtered, and the solvent removed in a rotary evaporator under reduced pressure. Vacuum distillation yielded 9.2 g of pure p-trimethylsilylphenyl acrylate.

Aufarbeitung

  1. temperatureThe solution was warmed
  2. washAfter 11/2 hours, the solution was washed two times with 5 percent sodium carbonate in water
  3. customseparated
  4. washAfter washing with brine
  5. customseparating
  6. dry with materialthe organic phase was dried over magnesium sulfate
  7. filtrationfiltered
  8. customthe solvent removed in a rotary evaporator under reduced pressure
  9. distillationVacuum distillation

Quellen und Nachweise

ORD-Eintrag
ord-0130afa88989486ea49d5a69d9c4a3f1
Quelldatensatz
uspto-grants-1983_08
Patentnummer
US04396704

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