m-Chloroperbenzoic acid → HCID 19805451, Verbindung

HRID 1681694Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1681694
ClC1C=CC=C(C(OO)=[O:9])C=1.[CH2:12]([S:16][C:17]1[CH:22]=[CH:21][C:20]([N:23]2[C:31](=[O:32])[C:30]3[C:25](=[CH:26][CH:27]=[CH:28][CH:29]=3)[NH:24]2)=[CH:19][CH:18]=1)[CH2:13][CH2:14][CH3:15]>C(Cl)Cl>[CH2:12]([S:16]([C:17]1[CH:18]=[CH:19][C:20]([N:23]2[C:31](=[O:32])[C:30]3[C:25](=[CH:26][CH:27]=[CH:28][CH:29]=3)[NH:24]2)=[CH:21][CH:22]=1)=[O:9])[CH2:13][CH2:14][CH3:15]

Komponenten

4

Edukt 2

HCID 70297m-Chloroperbenzoic acidHCID 54375321HCID 54375321, Verbindung

Produkt 1

HCID 19805451HCID 19805451, VerbindungAusbeute 60,7 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

3-Chloroperbenzoic acid (150mg) was added to a stirred solution of 1,2-dihydro-2-(4-butylthiophenyl)-3H-indazol-3-one (250 mg) in methylene chloride (5 ml) at 0-5° C. Stirring was continued for 15 minutes after the addition was complete. The reaction mixture was then washed with water, dried (MgSO4) and evaporated in vacuo. The residue was purified by column chromatography using methylene chloride/ether (70:30 v/v) to give 1,2-dihydro-2-(4-butylsulphinylphenyl)-3H-indazol-3-one (Ex. 52) as a solid (160 mg), m.p. 168-169° C.

Aufarbeitung

  1. additionafter the addition
  2. washThe reaction mixture was then washed with water
  3. dry with materialdried (MgSO4)
  4. customevaporated in vacuo
  5. customThe residue was purified by column chromatography

Quellen und Nachweise

ORD-Eintrag
ord-8aa3f413e504493cacde6135f1e06f09
Quelldatensatz
uspto-grants-1992_12
Patentnummer
US05173496

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