Hydrochloric Acid → HCID 21867183, Verbindung

HRID 857126Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 857126
[I:1][C:2]1[CH:3]=[C:4]([N:8]2[CH2:12][C:11](=[O:13])[NH:10][C:9]2=[O:14])[CH:5]=[CH:6][CH:7]=1.[H-].[Na+].[CH2:17](Br)[C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1.Cl>CN(C=O)C>[CH2:17]([N:10]1[C:11](=[O:13])[CH2:12][N:8]([C:4]2[CH:5]=[CH:6][CH:7]=[C:2]([I:1])[CH:3]=2)[C:9]1=[O:14])[C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1

Komponenten

6

Edukt 4

HCID 313Hydrochloric AcidHCID 7498Benzyl BromideHCID 24758Sodium hydrideHCID 218671771-(3-Iodophenyl)-2,4-imidazolidinedione

Produkt 1

HCID 21867183HCID 21867183, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel

Versuchsvorschrift

1-(3-Iodophenyl)imidazolidine-2,4-dione (0.5 g) was taken up in dry DMF (10 ml) and treated with sodium hydride (60% oil dispersion, 73 mg) and stirred for 20 min under nitrogen. Benzyl bromide (0.295 ml) was added and stirring continued for 3 h. 2M HCl (100 ml) was added and the mixture extracted with EtOAc. The combined extracts were washed with saturated aqueous sodium hydrogen carbonate (50 ml), brine (50 ml) and dried (MgSO4). This was recrystallised from MeOH to give the title compound (0.255 g). LCMS RT 3.53 min.

Aufarbeitung

  1. stirringstirring
  2. waitcontinued for 3 h
  3. extractionthe mixture extracted with EtOAc
  4. washThe combined extracts were washed with saturated aqueous sodium hydrogen carbonate (50 ml), brine (50 ml)
  5. dry with materialdried (MgSO4)
  6. customThis was recrystallised from MeOH

Quellen und Nachweise

ORD-Eintrag
ord-dcd6f19d0f474d478dc5b878332a5e60
Quelldatensatz
uspto-grants-2006_12
Patentnummer
US07144908B2

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