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Acetic Acid → HCID 21464431, Verbindung

HRID 1940930
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1940930
[F:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([F:8])[C:3]=1[NH:9][S:10]([C:13]1[N:24]=[C:16]2[C:17]([O:22][CH3:23])=[CH:18][CH:19]=[C:20](Cl)[N:15]2[N:14]=1)(=[O:12])=[O:11].C[O-].[Na+].CS(C)=O.[C:32](O)(=[O:34])C>ClCCl.O>[F:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([F:8])[C:3]=1[NH:9][S:10]([C:13]1[N:24]=[C:16]2[C:17]([O:22][CH3:23])=[CH:18][CH:19]=[C:20]([O:34][CH3:32])[N:15]2[N:14]=1)(=[O:12])=[O:11]
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

7

Edukt 4

HCID 176Acetic AcidHCID 679Dimethyl SulfoxideHCID 10942334Sodium MethoxideHCID 21464366HCID 21464366, Verbindung

Produkt 1

HCID 21464431HCID 21464431, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 962WaterLösungsmittel
HCID 6344DichloromethaneLösungsmittel

Reaktionsbedingungen

Temperatur
70 °C

Versuchsvorschrift

N-(2,6-Difluorophenyl)-5-chloro-8-methoxy[1,2,4]triazolo[1,5-a]pyridine-2-sulfonamide (1.0 g, 2.7 mmol), sodium methoxide (25 percent in methanol, 2.5 mL, 0.58 g, 11 mmol) and dimethyl sulfoxide (20 mL) were mixed with stirring and slowly heated to 70° C. over a 40-min period. After a short reaction period, the reaction mixture was acidified with acetic acid and diluted with dichloromethane and water. The solid that separated was recovered by filtration. The organic layer was separated, was washed several times with water, and was concentrated by evaporation under reduced pressure. The residue obtained was washed with water and combined with the previously obtained solid. The combined solids were washed with ether and hexane and dried to obtain 0.7 g of the title compound as an off-white powder melting at 319°-320° C. (d).

Aufarbeitung

  1. customAfter a short reaction period
  2. customThe solid that separated
  3. filtrationwas recovered by filtration
  4. customThe organic layer was separated
  5. washwas washed several times with water
  6. concentrationwas concentrated by evaporation under reduced pressure
  7. customThe residue obtained
  8. washwas washed with water
  9. washThe combined solids were washed with ether and hexane
  10. customdried

Quellen und Nachweise

ORD-Eintrag
ord-3e026fdd74094df2b592c41053dbfee6
Quelldatensatz
uspto-grants-1997_12
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US05700940

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