Butyryl chloride → HCID 19972830, Verbindung

HRID 1077431Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1077431
C(=O)([O-])[O-].[K+].[K+].[NH2:7][CH2:8][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.Br.[C:26](Cl)(=[O:30])[CH2:27][CH2:28][CH3:29]>O.C(OCC)(=O)C.O1CCCC1>[C:26]([NH:7][CH2:8][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:30])[CH2:27][CH2:28][CH3:29]

Komponenten

7

Edukt 3

HCID 8855Butyryl chlorideHCID 11430Potassium CarbonateHCID 214762912-aminomethyl-5-[pyridazin-3(2H)-on-6-yl]indane hydrobromide

Produkt 1

HCID 19972830HCID 19972830, VerbindungAusbeute 81,3 %

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 962WaterLösungsmittelHCID 8028TetrahydrofuranLösungsmittelHCID 8857Ethyl AcetateLösungsmittel

Versuchsvorschrift

An aqueous solution (100 ml) containing 3.30 g of potassium carbonate dissolved in water was added to 100 ml of a suspension containing 3.50 g of 2-aminomethyl-5-[pyridazin3(2H)-on-6-yl]indane·hydrobromide suspended in ethyl acetate. Then, under ice cooling, 2.30 g of butyryl chloride dissolved in 30 ml of tetrahydrofuran was added to the mixture, and the resulting mixture was stirred for 3 hours. Crystals precipitated were collected by filtration, washed with water, dried and then recrystallized from methanol to obtain 2.75 g of 2-(butyrylamino)methyl-5-[pyridazin-3(2H)-on-6-yl]indane.

Aufarbeitung

  1. additionwas added to the mixture
  2. customCrystals precipitated
  3. filtrationwere collected by filtration
  4. washwashed with water
  5. customdried
  6. customrecrystallized from methanol

Quellen und Nachweise

ORD-Eintrag
ord-7e5b8ebf50524b7885ebd32dd0e73e5f
Quelldatensatz
uspto-grants-1996_08
Patentnummer
US05543409

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