Hydrochloric Acid → HCID 67095239, Verbindung

HRID 2112077Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2112077
[N+:1]([C:4]1[CH:12]=[CH:11][CH:10]=[C:9]2[C:5]=1[C:6](=[O:13])[NH:7][NH:8]2)([O-:3])=[O:2].[CH3:14]I.Cl>CN(C)C(=O)C>[CH3:14][N:8]1[C:9]2[C:5](=[C:4]([N+:1]([O-:3])=[O:2])[CH:12]=[CH:11][CH:10]=2)[C:6](=[O:13])[NH:7]1

Komponenten

5

Edukt 3

HCID 313Hydrochloric AcidHCID 6328Methyl iodideHCID 247281924-Nitro-1,2-dihydro-3H-indazol-3-one

Produkt 1

HCID 67095239HCID 67095239, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 31374DimethylacetamideLösungsmittel

Versuchsvorschrift

306 mg (1.7 mmol) 4-nitro-1,2-dihydro-indazol-3-one are dissolved in 1 ml N,N-dimethyl-acetamide, combined with 150 μl (2.4 mmol) methyl iodide and 500 μl (2.32 mmol) of N-ethyldiisopropylamide and stirred for 2 h at ambient temperature. Then the reaction mixture is combined with 40 ml of a 1 N aqueous hydrochloric acid and extracted twice with 50 ml dichloromethane. Then the organic phase is dried with MgSO4, the solvent is eliminated in vacuo and the crude product is purified by chromatography. The carrier used is C18-RP-silica gel and a gradient is run through which consists of 95% water and 5% acetonitrile at the starting point and 5% water and 95% acetonitrile at the finishing point.

Aufarbeitung

  1. extractionextracted twice with 50 ml dichloromethane
  2. dry with materialThen the organic phase is dried with MgSO4
  3. customthe crude product is purified by chromatography

Quellen und Nachweise

ORD-Eintrag
ord-08a147b6f56d478990c0f87e92ca21e1
Quelldatensatz
uspto-grants-2009_04
Patentnummer
US07521457B2

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