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Phosphorus oxychloride → HCID 57743131, Verbindung

HRID 910137
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 910137
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[C:13]([CH3:14])=[N:12][NH:11][C:10](=O)[C:9]=2[C:16]2[CH:20]=[CH:19][S:18][CH:17]=2)=[CH:4][CH:3]=1.P(Cl)(Cl)([Cl:23])=O>>[Cl:23][C:10]1[N:11]=[N:12][C:13]([CH3:14])=[C:8]([C:5]2[CH:6]=[CH:7][C:2]([Cl:1])=[CH:3][CH:4]=2)[C:9]=1[C:16]1[CH:20]=[CH:19][S:18][CH:17]=1
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

3

Edukt 2

HCID 24813Phosphorus oxychlorideHCID 57743109HCID 57743109, Verbindung

Produkt 1

HCID 57743131HCID 57743131, Verbindung

Reaktionsbedingungen

Temperatur
110 °C

Versuchsvorschrift

1.38 g of 5-(4-chloro-phenyl)-6-methyl-4-(3-thienyl)-2H-pyridazin-3-on e and 6 ml of phosphorus oxychloride were mixed. The mixture was stirred for 1 hour on an oil bath of 110° C. The reaction mixture was allowed to cool to room temperature, then, concentrated under reduced pressure. To the resultant residue was added ethyl acetate and ice water. The mixture was stirred for about 5 minutes at room temperature, then, liquid-partitioned. The organic layer was washed with brine three times, and dried over anhydrous magnesium sulfate, then, concentrated under reduced pressure, to obtain 1.34 g of 3-chloro-5-(4-chlorophenyl)-6-methyl-4-(3-thienyl)pyridazine (hereinafter, described as compound (9) of the present invention.).

Aufarbeitung

  1. temperatureto cool to room temperature
  2. concentrationconcentrated under reduced pressure
  3. additionTo the resultant residue was added ethyl acetate and ice water
  4. stirringThe mixture was stirred for about 5 minutes at room temperature
  5. customliquid-partitioned
  6. washThe organic layer was washed with brine three times
  7. dry with materialdried over anhydrous magnesium sulfate
  8. concentrationconcentrated under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-0cabca25e0924a83add3a4e9d1978236
Quelldatensatz
uspto-grants-2011_09
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08022073B2

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