Triethylamine → HCID 21476308, Verbindung

HRID 2293105Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2293105
C(N(CC)CC)C.[NH2:8][CH2:9][CH:10]1[CH2:18][C:17]2[C:12](=[CH:13][CH:14]=[C:15]([C:19]3[CH2:20][CH2:21][C:22](=[O:25])[NH:23][N:24]=3)[CH:16]=2)[CH2:11]1.[CH2:26]([S:29](Cl)(=[O:31])=[O:30])[CH2:27][CH3:28]>CN1CCN(C)C1=O.O1CCCC1>[CH2:26]([S:29]([NH:8][CH2:9][CH:10]1[CH2:18][C:17]2[C:12](=[CH:13][CH:14]=[C:15]([C:19]3[CH2:20][CH2:21][C:22](=[O:25])[NH:23][N:24]=3)[CH:16]=2)[CH2:11]1)(=[O:31])=[O:30])[CH2:27][CH3:28]

Komponenten

6

Edukt 3

HCID 8471TriethylamineHCID 662791-Propanesulfonyl chlorideHCID 21476304HCID 21476304, Verbindung

Produkt 1

HCID 21476308HCID 21476308, VerbindungAusbeute 61,7 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 66611,3-Dimethyl-2-imidazolidinoneLösungsmittelHCID 8028TetrahydrofuranLösungsmittel

Versuchsvorschrift

5.53 g of triethylamine was added to 6.03 g of 2-aminomethyl-5-[4,5-dihydropyridazin-3(2H)-on-6-yl]indane suspended in 60 ml of 1,3-dimethyl-2-imidazolidinone, and then 5.10 g of propanesulfonyl chloride dissolved in 20 ml of tetrahydrofuran was added to the mixture. The resulting mixture was stirred at room temperature for 30 minutes. The reaction mixture was poured into ice water, and crystals precipitated were collected by filtration. The precipitated crystals were recrystallized from methanol-acetonitrile to obtain 5.34 g of 2-(propylsulfonylaminomethyl)-5-[4,5-dihydropyridazin-3(2H)-on-6-yl]indane

Aufarbeitung

  1. additionwas added to the mixture
  2. customprecipitated
  3. filtrationwere collected by filtration
  4. customThe precipitated crystals were recrystallized from methanol-acetonitrile

Quellen und Nachweise

ORD-Eintrag
ord-d04d03f739b44764a609e864c48331e4
Quelldatensatz
uspto-grants-1997_11
Patentnummer
US05686452

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