Acetic Acid → 1-tosyl-6,7-dihydro-1H-indazol-4(5H)-one

HRID 62447

Reaktionsgleichung

Reaktionsgleichung von HRID 62447
C[N:2]([CH:4]=[C:5]1[C:10](=O)[CH2:9][CH2:8][CH2:7][C:6]1=[O:12])C.[S:13]([NH:23]N)([C:16]1[CH:22]=[CH:21][C:19]([CH3:20])=[CH:18][CH:17]=1)(=[O:15])=[O:14].CC(O)=O>CCO>[S:13]([N:23]1[C:10]2[CH2:9][CH2:8][CH2:7][C:6](=[O:12])[C:5]=2[CH:4]=[N:2]1)([C:16]1[CH:22]=[CH:21][C:19]([CH3:20])=[CH:18][CH:17]=1)(=[O:15])=[O:14]

Komponenten

5

Edukt 3

HCID 176Acetic AcidHCID 15303P-ToluenesulfonylhydrazideHCID 3593532-[(Dimethylamino)methylidene]cyclohexane-1,3-dione

Produkt 1

HCID 674585881-tosyl-6,7-dihydro-1H-indazol-4(5H)-oneAusbeute 51,3 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Versuchsvorschrift

A solution of 2-((dimethylamino)methylene)cyclohexane-1,3-dione (55 g, 0.329 mol), 2-tosylhydrazine (61.3 g, 0.329 mol) and AcOH (33 mL) in EtOH (540 mL) was heated for 4 h at 70° C. Removed the solvent under reduced pressure and the residue was recrystallized using PE/EA=5/1 to give 1-tosyl-6,7-dihydro-1H-indazol-4(5H)-one (49 g, yield 51.3%) as a white solid.

Aufarbeitung

  1. customRemoved the solvent under reduced pressure
  2. customthe residue was recrystallized

Quellen und Nachweise

ORD-Eintrag
ord-ecfba064d9a14925a662eb32c5e86b69
Quelldatensatz
uspto-grants-2016_09
Patentnummer
US09446130B2

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