Water → HCID 22249795, Verbindung

HRID 966034Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 966034
[Br:1]Br.[O:3]1[C:7]([C:8]2[C:9]([CH3:26])=[N:10][N:11]3[C:16]4[N:17]([CH:20]([CH2:23][CH3:24])[CH2:21][CH3:22])[CH2:18][CH2:19][C:15]=4[C:14]([CH3:25])=[N:13][C:12]=23)=[CH:6][C:5]2[CH:27]=[CH:28][CH:29]=[CH:30][C:4]1=2.O>CN(C)C=O.C(OCC)(=O)C>[Br:1][C:6]1[C:5]2[CH:27]=[CH:28][CH:29]=[CH:30][C:4]=2[O:3][C:7]=1[C:8]1[C:9]([CH3:26])=[N:10][N:11]2[C:16]3[N:17]([CH:20]([CH2:21][CH3:22])[CH2:23][CH3:24])[CH2:18][CH2:19][C:15]=3[C:14]([CH3:25])=[N:13][C:12]=12

Komponenten

6

Edukt 3

HCID 962WaterHCID 24408BromineHCID 22249918HCID 22249918, Verbindung

Produkt 1

HCID 22249795HCID 22249795, VerbindungAusbeute 96,7 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 6228DimethylformamideLösungsmittelHCID 8857Ethyl AcetateLösungsmittel

Versuchsvorschrift

Bromine (1.0 M solution in carbon tetrachloride 0.3 mL, 0.30 mmol) was added to a solution of 3-benzo[b]furan-2-yl-8-(1-ethylpropyl)-2,5-dimethyl-7,8-dihydro-6H-pyrazolo[1,5-a]pyrrolo[3,2-e]pyrimidine (50 mg, 0.13 mmol) in N,N-dimethylformamide (0.3 mL) at 0° C., followed by stirring for one hour. Hypo water was added thereto, and the mixture was diluted with ethyl acetate, washed with an aqueous saturated solution of ammonium chloride and brine, dried over anhydrous magnesium sulfate and evaporated. The residue was purified by silica gel column chromatography (10% ethyl acetate/hexane), to give the title compound (57 mg) as white crystals.

Aufarbeitung

  1. washwashed with an aqueous saturated solution of ammonium chloride and brine
  2. dry with materialdried over anhydrous magnesium sulfate
  3. customevaporated
  4. customThe residue was purified by silica gel column chromatography (10% ethyl acetate/hexane)

Quellen und Nachweise

ORD-Eintrag
ord-8a19a511e5e84a68907b56a7efb24184
Quelldatensatz
uspto-grants-2005_10
Patentnummer
US06951865B2

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