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Ammonium Hydroxide → Ethyl 2-(3,5-bis(acetylamino)-2,4,6-triiodobenzoyloxy)butyrate

HRID 2379016
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 2379016
[CH3:1][C:2]([NH:4][C:5]1[C:10]([I:11])=[C:9]([NH:12][C:13]([CH3:15])=[O:14])[C:8]([I:16])=[C:7]([C:17]([O-:19])=[O:18])[C:6]=1[I:20])=[O:3].[Na+].Br[CH:23]([CH2:29][CH3:30])[C:24]([O:26][CH2:27][CH3:28])=[O:25].[OH-].[NH4+]>CN(C)C=O>[C:13]([NH:12][C:9]1[C:8]([I:16])=[C:7]([C:6]([I:20])=[C:5]([NH:4][C:2](=[O:3])[CH3:1])[C:10]=1[I:11])[C:17]([O:19][CH:23]([CH2:29][CH3:30])[C:24]([O:26][CH2:27][CH3:28])=[O:25])=[O:18])(=[O:14])[CH3:15]
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Komponenten

5

Edukt 3

HCID 14923Ammonium HydroxideHCID 79039Butanoic acid, 2-bromo-, ethyl esterHCID 23672589Sodium Amidotrizoate

Produkt 1

HCID 11377613Ethyl 2-(3,5-bis(acetylamino)-2,4,6-triiodobenzoyloxy)butyrateAusbeute 66,5 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel

Versuchsvorschrift

To 500 mL of dry N,N-dimethylformamide was added 159 g (0.250 mol) sodium diatrizoate and 54.5 g (0.280 mol) of ethyl 2-bromobutyrate. The mixture was heated on a steam bath for 20 h, cooled to room temperature and poured into 3 L of dilute ammonium hydroxide. The solid was filtered, washing with water, and air-dried. The solid was further purified by crystallization from 50% aqueous ethanol (after treatment with decolorizing carbon) affording two crops which were dried at 100° C. overnight to afford 121 g (66%) of a white powder, m.p. 288°-290° C. (dec.). Analysis for C17H19I3N2O6 : Calculated/Found: C, 28.05/28.36/H, 2.63/2.55; I, 52.3/52.3.

Aufarbeitung

  1. temperatureThe mixture was heated on a steam bath for 20 h
  2. filtrationThe solid was filtered
  3. washwashing with water
  4. customair-dried
  5. customThe solid was further purified by crystallization from 50% aqueous ethanol (after treatment with decolorizing carbon)
  6. customaffording two crops which
  7. customwere dried at 100° C. overnight

Quellen und Nachweise

ORD-Eintrag
ord-12d3352ce72747c6a256ffc9da6b5c14
Quelldatensatz
uspto-grants-1994_11
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US05360604

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