Citric Acid → HCID 59168188, Verbindung

HRID 1443954

Reaktionsgleichung

Reaktionsgleichung von HRID 1443954
[H-].[Na+].Br[C:4]1[C:5]([NH:11][S:12]([C:15]2[CH:20]=[CH:19][CH:18]=[C:17]([Cl:21])[C:16]=2[Cl:22])(=[O:14])=[O:13])=[N:6][CH:7]=[C:8]([CH3:10])[N:9]=1.[C:23]([OH:35])(=O)[CH2:24][C:25]([CH2:30][C:31]([OH:33])=O)(C(O)=O)O>COCCOC>[Cl:22][C:16]1[C:17]([Cl:21])=[CH:18][CH:19]=[CH:20][C:15]=1[S:12]([NH:11][C:5]1[C:4]([O:33][CH2:31][C:30]2[O:35][CH:23]=[CH:24][CH:25]=2)=[N:9][C:8]([CH3:10])=[CH:7][N:6]=1)(=[O:14])=[O:13]

Komponenten

5

Edukt 3

HCID 311Citric AcidHCID 24758Sodium hydrideHCID 59168147N-(3-Bromo-5-methyl-2-pyrazinyl)-2,3-dichlorobenzenesulphonamide

Produkt 1

HCID 59168188HCID 59168188, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 80711,2-DimethoxyethaneLösungsmittel

Reaktionsbedingungen

Temperatur
40 °C

Versuchsvorschrift

Sodium hydride (0.04 g of a 60% dispersion in oil) was added to fi rylalcohol (0.034 g) in 1,2-dimethoxyethane (1 mL). After 5 minutes N-(3-Bromo-5-methyl-2-pyrazinyl)-2,3-dichlorobenzenesulphonamide (Example 20 part a) (0.1 g) was added and the mixture heated at 40° C. After 16 h, 5% aqueous citric acid (10 mL) was added and the mixture extracted with ethyl acetate (2×50 mL). The combined extracts were washed with brine, dried (MgSO4) and the solvent evaporated. Chromatography on silica gel eluting with dichloromethane gave the title compound as a white solid (0.02 g)

Aufarbeitung

  1. extractionthe mixture extracted with ethyl acetate (2×50 mL)
  2. washThe combined extracts were washed with brine
  3. dry with materialdried (MgSO4)
  4. customthe solvent evaporated

Quellen und Nachweise

ORD-Eintrag
ord-0cb331558e224fd692f53ae09f63603a
Quelldatensatz
uspto-grants-2010_02
Patentnummer
US07662825B2

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