Dimethyl Sulfoxide → HCID 19972830, Verbindung

HRID 1077434Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1077434
Br.C(O)(=O)C.CS(C)=O.[C:10]([NH:15][CH2:16][CH:17]1[CH2:25][C:24]2[C:19](=[CH:20][CH:21]=[C:22]([C:26]3[CH2:27][CH2:28][C:29](=[O:32])[NH:30][N:31]=3)[CH:23]=2)[CH2:18]1)(=[O:14])[CH2:11][CH2:12][CH3:13].C(OC(C)C)(C)C>C(O)(=O)C>[C:10]([NH:15][CH2:16][CH:17]1[CH2:25][C:24]2[C:19](=[CH:20][CH:21]=[C:22]([C:26]3[CH:27]=[CH:28][C:29](=[O:32])[NH:30][N:31]=3)[CH:23]=2)[CH2:18]1)(=[O:14])[CH2:11][CH2:12][CH3:13]

Komponenten

6

Edukt 4

HCID 679Dimethyl SulfoxideHCID 7914Diisopropyl EtherHCID 19972832HCID 19972832, VerbindungHCID 21893785Acetic Acid Mixture with Hydrobromic Acid

Produkt 1

HCID 19972830HCID 19972830, VerbindungAusbeute 90 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 176Acetic AcidLösungsmittel

Versuchsvorschrift

25 ml of 30% hydrogen bromide-acetic acid and 1 ml of dimethyl sulfoxide were added to 20 ml of a suspension containing 3.13 g of 2-(butyrylamino)methyl-5-[4,5-di-hydropyridazin-3(2H)-on-6-yl]indane suspended in acetic acid. The mixture was stirred at room temperature for 3 hours. Diisopropyl ether was added to the mixture, and crystals precipitated were collected by filtration, washed with water, dried and then recrystallized from methanol to obtain 2.80 g of 2-(butyrylamino)methyl-5-[pyridazin-3(2H)-on-6-yl]indane.

Aufarbeitung

  1. customprecipitated
  2. filtrationwere collected by filtration
  3. washwashed with water
  4. customdried
  5. customrecrystallized from methanol

Quellen und Nachweise

ORD-Eintrag
ord-105a1d34bf06415989b1368bc46c7d13
Quelldatensatz
uspto-grants-1996_08
Patentnummer
US05543409

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