Hydrochloric Acid → 6,7-Dichloro-5-(4-pyridyl)-2,3(1H,4H)-quinoxalinedione

HRID 842657Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 842657
[Cl:1][C:2]1[C:3]([C:17]2[CH:22]=[CH:21][N:20]=[CH:19][CH:18]=2)=[C:4]2[C:9](=[CH:10][C:11]=1[Cl:12])[N:8]=[C:7]([O:13]C)[C:6]([O:15]C)=[N:5]2.Cl>O1CCOCC1>[Cl:1][C:2]1[C:3]([C:17]2[CH:22]=[CH:21][N:20]=[CH:19][CH:18]=2)=[C:4]2[C:9](=[CH:10][C:11]=1[Cl:12])[NH:8][C:7](=[O:13])[C:6](=[O:15])[NH:5]2

Komponenten

4

Edukt 2

HCID 313Hydrochloric AcidHCID 108606436,7-Dichloro-2,3-dimethoxy-5-(4-pyridyl)quinoxaline

Produkt 1

HCID 110667836,7-Dichloro-5-(4-pyridyl)-2,3(1H,4H)-quinoxalinedioneAusbeute 17 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 312751,4-DioxaneLösungsmittel

Versuchsvorschrift

A mixture of 6,7-dichloro-2,3-dimethoxy-5-(4-pyridyl)quinoxaline (Preparation 2, 110 mg, 0.327 mmol), 2M aqueous hydrochloric acid solution (1 mL) and 1,4-dioxane (7 ml) was heated under reflux for 2 hours, cooled, and concentrated under reduced pressure. The solid residue was triturated with water, collected by filtration and washed with water and diethyl ether to give the title compound (17 mg, 17%) as a white solid, mp >300° C.

Aufarbeitung

  1. temperaturewas heated
  2. temperatureunder reflux for 2 hours
  3. temperaturecooled
  4. concentrationconcentrated under reduced pressure
  5. customThe solid residue was triturated with water
  6. filtrationcollected by filtration
  7. washwashed with water and diethyl ether

Quellen und Nachweise

ORD-Eintrag
ord-877203458497448cb537e1c25866f628
Quelldatensatz
uspto-grants-2002_04
Patentnummer
US06376490B1

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