Hydrochloric Acid → N-(1.4-Dihydro-6.7-dichloro-2.3-dioxoquinoxaline-5-yl)-N-(3-pyridylmethyl)methanesulphonamide hydrochloride

HRID 1458556Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1458556
[Cl:1][C:2]1[C:3]([N:17]([CH2:22][C:23]2[CH:24]=[N:25][CH:26]=[CH:27][CH:28]=2)[S:18]([CH3:21])(=[O:20])=[O:19])=[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>[ClH:1].[Cl:1][C:2]1[C:3]([N:17]([CH2:22][C:23]2[CH:24]=[N:25][CH:26]=[CH:27][CH:28]=2)[S:18]([CH3:21])(=[O:20])=[O:19])=[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 22097013N-(6,7-dichloro-2,3-dimethoxyquinoxalin-5-yl)-N-(3-pyridylmethyl)methanesulphonamide

Produkt 1

HCID 22097005N-(1.4-Dihydro-6.7-dichloro-2.3-dioxoquinoxaline-5-yl)-N-(3-pyridylmethyl)methanesulphonamide hydrochlorideAusbeute 181,3 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 312751,4-DioxaneLösungsmittel

Versuchsvorschrift

A mixture of N-(6,7-dichloro-2,3-dimethoxyquinoxalin-5-yl)-N-(3-pyridylmethyl)-methanesulphonamide (130 mg, 0.293 mmol), 2M hydrochloric acid (2 ml) and dioxane (4 ml) was heated at reflux for 2.5 hours, cooled, and concentrated under reduced pressure. The residue was suspended in water (1 ml), filtered off, and washed with water and ether to give the title compound (120 mg, 98%) as a white solid, m.p. 234°-235° C. (dec.).

Aufarbeitung

  1. temperaturewas heated
  2. temperatureat reflux for 2.5 hours
  3. temperaturecooled
  4. concentrationconcentrated under reduced pressure
  5. filtrationfiltered off
  6. washwashed with water and ether

Quellen und Nachweise

ORD-Eintrag
ord-115a64dcec294303b602f2f6f711fc17
Quelldatensatz
uspto-grants-1998_12
Patentnummer
US05852016

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