Water → HCID 14625291, Verbindung

HRID 1073677Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1073677
[Cl:1][C:2]1[N:3]([C:11]2[CH:16]=[C:15]([N+:17]([O-:19])=[O:18])[C:14](F)=[CH:13][C:12]=2[F:21])[N:4]=[C:5]2[C:10]=1[CH2:9][CH2:8][CH2:7][CH2:6]2.[CH3:22][CH2:23][CH2:24][CH2:25][O:26][C:27]([CH2:29][OH:30])=[O:28].[F-].[K+].O>O1CCOCC1>[Cl:1][C:2]1[N:3]([C:11]2[CH:16]=[C:15]([N+:17]([O-:19])=[O:18])[C:14]([O:30][CH2:29][C:27]([O:26][CH2:25][CH2:24][CH2:23][CH3:22])=[O:28])=[CH:13][C:12]=2[F:21])[N:4]=[C:5]2[C:10]=1[CH2:9][CH2:8][CH2:7][CH2:6]2

Komponenten

6

Edukt 4

HCID 962WaterHCID 81882Butyl GlycolateHCID 522689Potassium FluorideHCID 14625290HCID 14625290, Verbindung

Produkt 1

HCID 14625291HCID 14625291, VerbindungAusbeute 75,1 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 312751,4-DioxaneLösungsmittel

Versuchsvorschrift

A suspension of 3-chloro-2-(2,4-difluoro-5-nitrophenyl)-4,5,6,7-tetrahydro-2H-indazole (10 g), butyl glycollate (5 g) and potassium fluoride (10 g) in dioxane (30 g) was refluxed for 1 hour. After completion of the reaction, the reaction mixture was poured into water and extracted with ethyl acetate. The extract was dried over magnesium sulfate and concentrated. The residue was purified by liquid column chromatography using a mixture of hexane and ethyl acetate as an eluent to give 3-chloro-2-(2-fluoro-4-butyloxycarbonylmethoxy-5-nitro-phenyl)-4,5,6,7-tetrahydro-2H-indazole (10.2 g). m.p., 138°-139° C.

Aufarbeitung

  1. temperaturewas refluxed for 1 hour
  2. customAfter completion of the reaction
  3. extractionextracted with ethyl acetate
  4. dry with materialThe extract was dried over magnesium sulfate
  5. concentrationconcentrated
  6. customThe residue was purified by liquid column chromatography
  7. additiona mixture of hexane and ethyl acetate as an eluent

Quellen und Nachweise

ORD-Eintrag
ord-e420d9b7d1874a5db31ea6443ee79659
Quelldatensatz
uspto-grants-1990_11
Patentnummer
US04970322

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