Triethylamine → HCID 178488163, Verbindung

HRID 357553Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 357553
[OH:1][CH2:2][CH2:3][O:4][C:5]1[CH:10]=[CH:9][N:8]=[C:7]([CH2:11][S:12][C:13]2[NH:17][C:16]3[CH:18]=[CH:19][C:20]([O:22][CH3:23])=[CH:21][C:15]=3[N:14]=2)[C:6]=1[CH3:24].ClC1C=CC=C(C(OO)=[O:33])C=1.C(N(CC)CC)C.C(=O)([O-])O.[Na+]>CO.ClCCl>[OH:1][CH2:2][CH2:3][O:4][C:5]1[CH:10]=[CH:9][N:8]=[C:7]([CH2:11][S:12]([C:13]2[NH:17][C:16]3[CH:18]=[CH:19][C:20]([O:22][CH3:23])=[CH:21][C:15]=3[N:14]=2)=[O:33])[C:6]=1[CH3:24]

Komponenten

7

Edukt 4

HCID 8471TriethylamineHCID 70297m-Chloroperbenzoic acidHCID 516892Sodium BicarbonateHCID 178488131HCID 178488131, Verbindung

Produkt 1

HCID 178488163HCID 178488163, VerbindungAusbeute 61,6 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 887MethanolLösungsmittelHCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

0.9 g of 2-[4-(2-hydroxyethoxy)-3-methylpyridine-2-yl]methylthio-5-methoxy-1H-benzimidazole was dissolved in a mixture comprising 5 ml of methanol and 80 ml of dichloromethane to obtain a solution. 0.51 g of m-chloroperbenzoic acid was added to this solution at -60° C. The obtained mixture was stirred at -50° to -40° C. for 4.5 hours, followed by the addition of 0.38 g of triethylamine. A saturated aqueous solution of sodium hydrogencarbonate was added to the obtained mixture and the resulting mixture was extracted with chloroform. The extract was dried over magnesium sulfate and filtered. The filtrate was distilled under a reduced pressure to obtain a crude product. This crude product was crystallized from dichloromethane/isopropyl ether to obtain 0.58 g of the title compound.

Aufarbeitung

  1. customto obtain a solution
  2. extractionthe resulting mixture was extracted with chloroform
  3. dry with materialThe extract was dried over magnesium sulfate
  4. filtrationfiltered
  5. distillationThe filtrate was distilled under a reduced pressure
  6. customto obtain a crude product
  7. customThis crude product was crystallized from dichloromethane/isopropyl ether

Quellen und Nachweise

ORD-Eintrag
ord-99f97f5a9dbe4073863cc3e493b3f8a4
Quelldatensatz
uspto-grants-1998_11
Patentnummer
US05840910

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