1H-Pyrazole, 4,5-dihydro-3-methyl-5-phenyl- → HCID 19873525, Verbindung

HRID 465282Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 465282
[CH3:1][N:2]([O:21][CH3:22])[S:3]([N:6]([S:8]([NH:11][C:12](=O)[O:13]C1C=CC=CC=1)(=[O:10])=[O:9])[CH3:7])(=[O:5])=[O:4].[CH3:23][C:24]1[CH2:28][CH:27]([C:29]2[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=2)[NH:26][N:25]=1>C1C=CC=CC=1>[CH3:1][N:2]([O:21][CH3:22])[S:3]([N:6]([S:8]([NH:11][C:12]([N:26]1[CH:27]([C:29]2[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=2)[CH2:28][C:24]([CH3:23])=[N:25]1)=[O:13])(=[O:9])=[O:10])[CH3:7])(=[O:5])=[O:4]

Komponenten

4

Edukt 2

HCID 101301011H-Pyrazole, 4,5-dihydro-3-methyl-5-phenyl-HCID 19873523HCID 19873523, Verbindung

Produkt 1

HCID 19873525HCID 19873525, VerbindungAusbeute 42,4 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 241BenzeneLösungsmittel

Versuchsvorschrift

A mixture comprising 1 g (2.83 mmol) of phenyl N-[(N-(N-methyl-N-methoxyaminosulfonyl)-N-methylamino)sulfonyl]-carbamate, 0.45 g (2.81 mmol) of 3-methyl-5-phenyl-2-pyrazoline and 30 ml of dry benzene was heated at 80° C. for 5 minutes. The mixture was left to cool, and then the solvent was distilled off under reduced pressure. The residue was purified by reverse phase column chromatography (CH3CN: H2O=7:3) to obtain 0.5 g of the desired 1-[(N-(N-methyl-N-methoxyaminosulfonyl)-N-methyl-amino)sulfonylcarbamoyl]-3-methyl-5-phenyl-2-pyrazoline as glassy substance.

Aufarbeitung

  1. waitThe mixture was left
  2. temperatureto cool
  3. distillationthe solvent was distilled off under reduced pressure
  4. customThe residue was purified by reverse phase column chromatography (CH3CN: H2O=7:3)

Quellen und Nachweise

ORD-Eintrag
ord-f2648dc302094aa992468d9ac0ed9dba
Quelldatensatz
uspto-grants-1992_10
Patentnummer
US05152824

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