Phosphorus oxychloride → HCID 19375606, Verbindung

HRID 2211101Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2211101
[S:1]1[CH:5]=[CH:4][C:3]([C:6]2[C:15]3[C:10](=[CH:11][CH:12]=[CH:13][CH:14]=3)[C:9](=O)[NH:8][N:7]=2)=[CH:2]1.P(Cl)(Cl)([Cl:19])=O>ClC(Cl)C>[Cl:19][C:9]1[C:10]2[C:15](=[CH:14][CH:13]=[CH:12][CH:11]=2)[C:6]([C:3]2[CH:4]=[CH:5][S:1][CH:2]=2)=[N:7][N:8]=1

Komponenten

4

Edukt 2

HCID 24813Phosphorus oxychlorideHCID 19375607HCID 19375607, Verbindung

Produkt 1

HCID 19375606HCID 19375606, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 63651,1-DichloroethaneLösungsmittel

Reaktionsbedingungen

Temperatur
100 °C

Versuchsvorschrift

500 mg of 4-(3-thienyl)-1-phthalazinone and 3 ml of phosphorus oxychloride were dissolved in 6 ml of dichloroethane, and the solution was stirred at 100° C. for 4 hours. The reaction solution was distilled off, and a 1-N aqueous NaOH solution was added thereto under cooling with ice. The solution was extracted with chloroform and dried over magnesium sulfide. The solvent was then distilled off, thereby obtaining 515 mg of 1-chloro-4-(3-thienyl)phthalazine.

Aufarbeitung

  1. distillationThe reaction solution was distilled off
  2. additiona 1-N aqueous NaOH solution was added
  3. temperatureunder cooling with ice
  4. extractionThe solution was extracted with chloroform
  5. dry with materialdried over magnesium sulfide
  6. distillationThe solvent was then distilled off

Quellen und Nachweise

ORD-Eintrag
ord-70d91eeaabdc4a6bb4faa7d1f9c5bdd3
Quelldatensatz
uspto-grants-1995_10
Patentnummer
US05462941

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