Triethylamine → HCID 59574484, Verbindung

HRID 2092109Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2092109
[Cl:1][C:2]1[C:3](=[O:23])[N:4]([CH2:9][C:10]([C:12]2[CH:17]=[CH:16][C:15]([N:18]([CH2:21][CH3:22])[CH2:19][CH3:20])=[CH:14][CH:13]=2)=[O:11])[N:5]=[CH:6][C:7]=1Cl.[CH2:24]1[CH:31]2[C:27]3([NH2:33])[CH2:28][CH:29]([CH2:32][CH:25]1[CH2:26]3)[CH2:30]2.C(N(CC)CC)C.[Cl-].[NH4+]>CN(C)C(=O)C>[Cl:1][C:2]1[C:3](=[O:23])[N:4]([CH2:9][C:10]([C:12]2[CH:17]=[CH:16][C:15]([N:18]([CH2:21][CH3:22])[CH2:19][CH3:20])=[CH:14][CH:13]=2)=[O:11])[N:5]=[CH:6][C:7]=1[NH:33][C:27]12[CH2:28][CH:29]3[CH2:32][CH:25]([CH2:24][CH:31]1[CH2:30]3)[CH2:26]2

Komponenten

6

Edukt 4

HCID 8471TriethylamineHCID 25517Ammonium ChlorideHCID 2794246HCID 2794246, VerbindungHCID 59574171HCID 59574171, Verbindung

Produkt 1

HCID 59574484HCID 59574484, VerbindungAusbeute 18,2 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 31374DimethylacetamideLösungsmittel

Versuchsvorschrift

4,5-Dichloro-2-{2-[4-(diethylamino)phenyl]-2-oxoethyl}pyridazin-3(2H)-one (30 mg, 0.0846 mmol), hexahydro-2,5-methanopentalen-3a(1H)-amine (22 mg, 0.126 mmol) and triethylamine (59 μL, 0.423 mmol) were stirred in N,N-dimethylacetamide (1 mL) at 90° C. for 3 days. After completion of the reaction, the reaction solution was mixed with aqueous ammonium chloride and extracted with ethyl acetate. The extract was dried over anhydrous magnesium sulfate and evaporated under reduced pressure. The resulting residue was purified by silica gel column chromatography (ethyl acetate/hexane=1/1) to give the desired product (7 mg, 17% yield).

Aufarbeitung

  1. customAfter completion of the reaction
  2. extractionextracted with ethyl acetate
  3. dry with materialThe extract was dried over anhydrous magnesium sulfate
  4. customevaporated under reduced pressure
  5. customThe resulting residue was purified by silica gel column chromatography (ethyl acetate/hexane=1/1)

Quellen und Nachweise

ORD-Eintrag
ord-5c31bf45506047158f41abdd90ecf857
Quelldatensatz
uspto-grants-2013_05
Patentnummer
US08440666B2

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