Water → HCID 178527559, Verbindung

HRID 1740997Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1740997
[NH2:1][C:2]1[C:6]([C:7]2[CH:12]=[CH:11][CH:10]=[CH:9][N:8]=2)=[C:5]([S:13][CH2:14][C:15]2[CH:20]=[CH:19][CH:18]=[C:17]([O:21][C:22]3[CH:27]=[CH:26][C:25]([F:28])=[CH:24][CH:23]=3)[CH:16]=2)[NH:4][N:3]=1.[Cl:29][C:30]1[CH:35]=[CH:34][CH:33]=[C:32]([Cl:36])[C:31]=1[S:37](Cl)(=[O:39])=[O:38].O>N1C=CC=CC=1>[Cl:29][C:30]1[CH:35]=[CH:34][CH:33]=[C:32]([Cl:36])[C:31]=1[S:37]([NH:1][C:2]1[C:6]([C:7]2[CH:12]=[CH:11][CH:10]=[CH:9][N:8]=2)=[C:5]([S:13][CH2:14][C:15]2[CH:20]=[CH:19][CH:18]=[C:17]([O:21][C:22]3[CH:23]=[CH:24][C:25]([F:28])=[CH:26][CH:27]=3)[CH:16]=2)[NH:4][N:3]=1)(=[O:39])=[O:38]

Komponenten

5

Edukt 3

HCID 962WaterHCID 5221832,6-DichlorobenzenesulfonylchlorideHCID 178509293HCID 178509293, Verbindung

Produkt 1

HCID 178527559HCID 178527559, VerbindungAusbeute 53,7 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1049PyridineLösungsmittel

Versuchsvorschrift

3-Amino-4-(2-pyridyl)-5-(3-(4-fluorophenoxy)benzylthio)-(1H)-pyrazole (0.39 g, 0.99 mmol) was dissolved in 5 ml of pyridine. Commercial 2,6-dichlorobenzenesulfonyl chloride (0.26 g, 1.04 mmol) was added and the red solution was stirred overnight at room temperature. The reaction mixture was poured into 50 ml of water and was extracted twice with 100 ml portions of ethyl acetate. The organic layers were washed with water and brine, combined, dried over MgSO4 and concentrated. The crude product was slurried in cold ethyl acetate and the solid was filtered off and washed with small portions of cold ethyl acetate and cold diethyl ether and dried under vacuum to afford 0.32 g (53% yield) of the final compound.

Aufarbeitung

  1. extractionwas extracted twice with 100 ml portions of ethyl acetate
  2. washThe organic layers were washed with water and brine
  3. dry with materialdried over MgSO4
  4. concentrationconcentrated
  5. filtrationthe solid was filtered off
  6. washwashed with small portions of cold ethyl acetate and cold diethyl ether
  7. customdried under vacuum

Quellen und Nachweise

ORD-Eintrag
ord-f41f426eeca54d00ae9fbc53b55e4f30
Quelldatensatz
uspto-grants-1999_10
Patentnummer
US05972972

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