m-Chloroperbenzoic acid → HCID 178493774, Verbindung

HRID 845514Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 845514
[CH3:1][O:2][C:3]1[C:8]([O:9][CH3:10])=[CH:7][N:6]=[C:5]([CH2:11][S:12][C:13]2[NH:17][C:16]3[CH:18]=[CH:19][C:20]([O:22][C:23]([F:28])([F:27])[CH:24]([F:26])[F:25])=[CH:21][C:15]=3[N:14]=2)[CH:4]=1.ClC1C=C(C=CC=1)C(OO)=[O:34]>C(Cl)Cl>[CH3:1][O:2][C:3]1[C:8]([O:9][CH3:10])=[CH:7][N:6]=[C:5]([CH2:11][S:12]([C:13]2[NH:17][C:16]3[CH:18]=[CH:19][C:20]([O:22][C:23]([F:27])([F:28])[CH:24]([F:25])[F:26])=[CH:21][C:15]=3[N:14]=2)=[O:34])[CH:4]=1

Komponenten

4

Edukt 2

HCID 70297m-Chloroperbenzoic acidHCID 178493768HCID 178493768, Verbindung

Produkt 1

HCID 178493774HCID 178493774, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel2×

Versuchsvorschrift

A solution of the product in methylene chloride is obtained by the procedure described in Example 2 by oxidation of 0.76 g of 2-[(4,5-dimethoxy-2-pyridyl)methylthio]-5-(1,1,2,2-tetrafluoroethoxy)-1H-benzimidazole with 19 ml of a 0.1M solution of m-chloroperoxybenzoic acid in 30 ml of methylene chloride at -40° C., after extraction. After drying the solution over magnesium sulfate, the drying agent is filtered off, the filtrate is concentrated and the residue is crystallized from methylene chloride/diisopropyl ether. 0.64 g (82% of theory) of the title compound is obtained in the form of colorless crystals of m.p. 160°-162° C. (decomp.).

Aufarbeitung

  1. extractionafter extraction
  2. dry with materialAfter drying the solution over magnesium sulfate
  3. filtrationthe drying agent is filtered off
  4. concentrationthe filtrate is concentrated
  5. customthe residue is crystallized from methylene chloride/diisopropyl ether

Quellen und Nachweise

ORD-Eintrag
ord-fb452fa10f6f47d1b71b3a9855095567
Quelldatensatz
uspto-grants-1988_07
Patentnummer
US04758579

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