Hydrochloric Acid → 2-n-butylsulfonylamino-5-[pyridazin-3(2H)-on-6-yl]indane

HRID 1598569

Reaktionsgleichung

Reaktionsgleichung von HRID 1598569
[CH2:1]([S:5]([NH:8][CH:9]1[CH2:17][C:16]2[C:11](=[CH:12][CH:13]=[C:14]([C:18]3[CH2:19][CH2:20][C:21](=[O:24])[NH:22][N:23]=3)[CH:15]=2)[CH2:10]1)(=[O:7])=[O:6])[CH2:2][CH2:3][CH3:4].[OH-].[Na+].[N+](C1C=C(S([O-])(=O)=O)C=CC=1)([O-])=O.[Na+].Cl>O>[CH2:1]([S:5]([NH:8][CH:9]1[CH2:17][C:16]2[C:11](=[CH:12][CH:13]=[C:14]([C:18]3[CH:19]=[CH:20][C:21](=[O:24])[NH:22][N:23]=3)[CH:15]=2)[CH2:10]1)(=[O:6])=[O:7])[CH2:2][CH2:3][CH3:4]

Komponenten

6

Edukt 4

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 31389Sodium 3-nitrobenzenesulfonateHCID 189297852-n-butylsulfonylamino-5-[4,5-dihydropyridazin-3(2H)-on-6-yl]indane

Produkt 1

HCID 189298022-n-butylsulfonylamino-5-[pyridazin-3(2H)-on-6-yl]indaneAusbeute 66,5 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

In 55 ml of water were dissolved 2.45 g of 2-n-butylsulfonylamino-5-[4,5-dihydropyridazin-3(2H)-on-6-yl]indane and 1.40 g of sodium hydroxide, and 2.66 g of sodium 3-nitrobenzenesulfonate was added thereto. The mixture was refluxed under heating for 5 hours. After cooling, the reaction mixture was made acidic with 10% hydrochloric acid and extracted with ethyl acetate, the extract was dried, and then the solvent was removed. The resulting crystals were recrystallized from methanol to obtain 1.62 g of 2-n-butylsulfonylamino-5-[pyridazin-3(2H)-on-6-yl]-indane.

Aufarbeitung

  1. additionwas added
  2. temperatureThe mixture was refluxed
  3. temperatureunder heating for 5 hours
  4. temperatureAfter cooling
  5. extractionextracted with ethyl acetate
  6. customthe extract was dried
  7. customthe solvent was removed
  8. customThe resulting crystals were recrystallized from methanol

Quellen und Nachweise

ORD-Eintrag
ord-3c945ea507404257b2fb5ee33d929fd4
Quelldatensatz
uspto-grants-1998_04
Patentnummer
US05739132

Verknüpfte Notizen

Wird geladen…