1,1'-Biphenyl, mixt. with 1,1'-oxybis(benzene) → HCID 178431852, Verbindung

HRID 911923Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 911923
C1C=CC(C2C=CC=CC=2)=CC=1.C1C=CC(OC2C=CC=CC=2)=CC=1.CC1(C)O[C:31](=[O:33])[C:30](=[CH:34][NH:35][C:36]2[C:40]([CH3:41])=[CH:39][S:38][CH:37]=2)C(=O)O1>>[CH3:41][C:40]1[C:36]2=[N:35][CH:34]=[CH:30][C:31]([OH:33])=[C:37]2[S:38][CH:39]=1

Komponenten

3

Edukt 2

HCID 246701,1'-Biphenyl, mixt. with 1,1'-oxybis(benzene)HCID 669953662,2-Dimethyl-5-((4-methylthiophen-3-ylamino)methylene)-1,3-dioxane-4,6-dione

Produkt 1

HCID 178431852HCID 178431852, VerbindungAusbeute 101,9 %

Reaktionsbedingungen

Temperatur
235 °C

Versuchsvorschrift

A solution of Dowtherm A (7 mL) was heated in oil bath at 235° C. under nitrogen. 2,2-dimethyl-5-((4-methylthiophen-3-ylamino)methylene)-1,3-dioxane-4,6-dione (5.0 g, 19 mmol) was added in portions over a 20 minutes period. After the last portion was added, the solution stirred at 235° C. for another 5 minutes. The solution was removed from the oil bath and allowed to cool to room temperature. Upon cooling, the product precipitated out of solution. Diethyl ether was added and the solid was filtered and dried to give the title compound (3.2 g) with residual amounts of Dowtherm A remaining.

Aufarbeitung

  1. additionAfter the last portion was added
  2. customThe solution was removed from the oil bath
  3. temperatureto cool to room temperature
  4. temperatureUpon cooling
  5. customthe product precipitated out of solution
  6. additionDiethyl ether was added
  7. filtrationthe solid was filtered
  8. customdried

Quellen und Nachweise

ORD-Eintrag
ord-539a958a87b240ed8fa6589d5c234605
Quelldatensatz
uspto-grants-2011_09
Patentnummer
US08022223B2

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