Acetic Acid → HCID 21464355, Verbindung

HRID 1898810Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1898810
C[O-].[Na+].CO.[Cl:6][C:7]1[CH:12]=[CH:11][CH:10]=[C:9]([Cl:13])[C:8]=1[NH:14][S:15]([C:18]1[N:28]=[C:21]2[CH:22]=[C:23]([Cl:27])[CH:24]=[C:25](Cl)[N:20]2[N:19]=1)(=[O:17])=[O:16].[C:29](O)(=[O:31])C>CS(C)=O.ClCCl.CCCCCC>[Cl:6][C:7]1[CH:12]=[CH:11][CH:10]=[C:9]([Cl:13])[C:8]=1[NH:14][S:15]([C:18]1[N:28]=[C:21]2[CH:22]=[C:23]([Cl:27])[CH:24]=[C:25]([O:31][CH3:29])[N:20]2[N:19]=1)(=[O:17])=[O:16]

Komponenten

8

Edukt 4

HCID 176Acetic AcidHCID 887MethanolHCID 10942334Sodium MethoxideHCID 21464351HCID 21464351, Verbindung

Produkt 1

HCID 21464355HCID 21464355, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 679Dimethyl SulfoxideLösungsmittelHCID 6344DichloromethaneLösungsmittelHCID 8058HexaneLösungsmittel

Versuchsvorschrift

Sodium methoxide in methanol (1.1 mL of 25 percent solution, 0.26 g, 0.005 mol) was added to a solution of N-(2,6-dichlorophenyl)-5,7-dichloro[1,2,4]triazolo[1,5-a]pyridine-2-sulfonamide (0.9 g, 0.02 mol) in dimethyl sulfoxide (30 mL) at ambient temperature with stirring. The reaction was complete in a few minutes, but was stirred for 30 min. The mixture was then acidified with acetic acid and diluted with dichloromethane. The resulting organic phase was recovered and washed with water and the volatiles were removed by evaporation under reduced pressure. The residue obtained was mixed with hexane and the insoluble solids were collected by filtration and dried to obtain 0.8 g (90 percent of theory) of the title compound as a light tan powder melting at 232°-234° C.(d).

Aufarbeitung

  1. waitThe reaction was complete in a few minutes
  2. stirringwas stirred for 30 min
  3. customThe resulting organic phase was recovered
  4. washwashed with water
  5. customthe volatiles were removed by evaporation under reduced pressure
  6. customThe residue obtained
  7. filtrationthe insoluble solids were collected by filtration
  8. customdried

Quellen und Nachweise

ORD-Eintrag
ord-ef84773e7d8c4636963a100d2533cc21
Quelldatensatz
uspto-grants-1996_11
Patentnummer
US05571775

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