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

HRID 1598567

Reaktionsgleichung

Reaktionsgleichung von HRID 1598567
[NH2:1][CH:2]1[CH2:10][C:9]2[C:4](=[CH:5][CH:6]=[C:7]([C:11]3[CH:12]=[CH:13][C:14](=[O:17])[NH:15][N:16]=3)[CH:8]=2)[CH2:3]1.C(N(CC)CC)C.[CH2:25]([S:29](Cl)(=[O:31])=[O:30])[CH2:26][CH2:27][CH3:28]>CN(C)C=O>[CH2:25]([S:29]([NH:1][CH:2]1[CH2:10][C:9]2[C:4](=[CH:5][CH:6]=[C:7]([C:11]3[CH:12]=[CH:13][C:14](=[O:17])[NH:15][N:16]=3)[CH:8]=2)[CH2:3]1)(=[O:31])=[O:30])[CH2:26][CH2:27][CH3:28]

Komponenten

5

Edukt 3

HCID 8471TriethylamineHCID 754301-Butanesulfonyl chlorideHCID 189297732-amino-5-[pyridazin-3(2H)-on-6-yl]indane

Produkt 1

HCID 189298022-n-butylsulfonylamino-5-[pyridazin-3(2H)-on-6-yl]indaneAusbeute 72,9 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel

Reaktionsbedingungen

Temperatur
50 °C

Versuchsvorschrift

In 50 ml of dimethylformamide were dissolved 1.14 g of 2-amino-5-[pyridazin-3(2H)-on-6-yl]indane and 0.8 g of triethyl amine, and 1.25 g of n-butanesulfonyl chloride was added thereto. The mixture was stirred at 50° C for 30 minutes and then stirred at room temperature overnight. The solvent was removed, water was added to the residue, and crystals precipitated were collected by filtration. The resulting crystals were recrystallized from methanol to obtain 1.27 g of 2-n-butylsulfonylamino-5-[pyridazin-3(2H)-on-6-yl]indane.

Aufarbeitung

  1. additionwas added
  2. stirringstirred at room temperature overnight
  3. customThe solvent was removed
  4. additionwater was added to the residue, and crystals
  5. customprecipitated
  6. filtrationwere collected by filtration
  7. customThe resulting crystals were recrystallized from methanol

Quellen und Nachweise

ORD-Eintrag
ord-5af222c59385436a96b3c24993006ea6
Quelldatensatz
uspto-grants-1998_04
Patentnummer
US05739132

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