Potassium Hydroxide → HCID 19805429, Verbindung

HRID 1681689

Reaktionsgleichung

Reaktionsgleichung von HRID 1681689
[N+:1]([C:4]1[CH:11]=[CH:10][C:7]([CH2:8]Br)=[CH:6][CH:5]=1)([O-:3])=[O:2].[C:12]([N:17]1[C:25]2[C:20](=[CH:21][CH:22]=[CH:23][CH:24]=2)[C:19](=[O:26])[NH:18]1)([O:14][CH2:15][CH3:16])=[O:13].[OH-].[K+]>C(O)C>[C:12]([N:17]1[C:25]2[C:20](=[CH:21][CH:22]=[CH:23][CH:24]=2)[C:19](=[O:26])[N:18]1[CH2:8][C:7]1[CH:10]=[CH:11][C:4]([N+:1]([O-:3])=[O:2])=[CH:5][CH:6]=1)([O:14][CH2:15][CH3:16])=[O:13]

Komponenten

5

Edukt 3

HCID 14797Potassium HydroxideHCID 660114-Nitrobenzyl bromideHCID 584113Ethyl 3-oxo-2,3-dihydro-1H-indazole-1-carboxylate

Produkt 1

HCID 19805429HCID 19805429, VerbindungAusbeute 59 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Versuchsvorschrift

4-Nitrobenzyl bromide (540 mg) was added to a mixture of 1,2-dihydro-1-carboethoxy-3H-indazol-3-one (206 mg) and potassium hydroxide (67 mg) in ethanol (10 ml). The mixture was heated under reflux for 30 minutes. The cooled solution was clarified by filtration and the filtrate was evaporated. The residue was purified by column chromatography using methylene chloride as eluant to give 1,2-dihydro-1-carboethoxy-2-(4-nitrobenzyl)-3H-indazol-3-one (Ex. 39) as a solid, m.p. 123-124° C. in 59% yield.

Aufarbeitung

  1. temperatureThe mixture was heated
  2. temperatureunder reflux for 30 minutes
  3. filtrationThe cooled solution was clarified by filtration
  4. customthe filtrate was evaporated
  5. customThe residue was purified by column chromatography

Quellen und Nachweise

ORD-Eintrag
ord-b5a0debec6f14606927ce7535fbf838d
Quelldatensatz
uspto-grants-1992_12
Patentnummer
US05173496

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