Hydrochloric Acid → 1-(1,4-Dihydro-6,7-dichloro-2,3-dioxoquinoxaline-5-yl)-3-butenyl methyl sulphone

HRID 1458564

Reaktionsgleichung

Reaktionsgleichung von HRID 1458564
[CH3:1][S:2]([CH:5]([C:9]1[C:18]([Cl:19])=[C:17]([Cl:20])[CH:16]=[C:15]2[C:10]=1[N:11]=[C:12]([O:23]C)[C:13]([O:21]C)=[N:14]2)[CH2:6][CH:7]=[CH2:8])(=[O:4])=[O:3].Cl>O1CCOCC1>[CH3:1][S:2]([CH:5]([C:9]1[C:18]([Cl:19])=[C:17]([Cl:20])[CH:16]=[C:15]2[C:10]=1[NH:11][C:12](=[O:23])[C:13](=[O:21])[NH:14]2)[CH2:6][CH:7]=[CH2:8])(=[O:3])=[O:4]

Komponenten

4

Edukt 2

HCID 313Hydrochloric AcidHCID 220970431-(6,7-Dichloro-2,3-dimethoxyquinoxalin-5-yl)-3-butenyl methyl sulphone

Produkt 1

HCID 220970101-(1,4-Dihydro-6,7-dichloro-2,3-dioxoquinoxaline-5-yl)-3-butenyl methyl sulphoneAusbeute 68 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 312751,4-DioxaneLösungsmittel

Reaktionsbedingungen

Temperatur
90 °C

Versuchsvorschrift

A mixture of 1-(6,7-dichloro-2,3-dimethoxyquinoxalin-5-yl)-3-butenyl methyl sulphone (from step (a), 27 mg, 0.069 mmol), 2M hydrochoric acid (0.5 ml) and dioxane (1 ml) was warmed at 90° C. for 15 h, cooled and concentrated under reduced pressure. The residue was sonicated with ether and a few drops of methanol and the resulting white solid was collected by filtration, washed with ether and dried to afford the title compound (17 mg, 68%) as a white powder, m.p. 270.5-272° C.

Aufarbeitung

  1. temperaturecooled
  2. concentrationconcentrated under reduced pressure
  3. customThe residue was sonicated with ether and a few drops of methanol
  4. filtrationthe resulting white solid was collected by filtration
  5. washwashed with ether
  6. customdried

Quellen und Nachweise

ORD-Eintrag
ord-44d65c2b3b014bd78ad7e756b87a67c7
Quelldatensatz
uspto-grants-1998_12
Patentnummer
US05852016

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