Potassium Iodide → HCID 11043631, Verbindung

HRID 2393513Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2393513
[C:1]([O:4][C:5]1[CH:21]=[CH:20][C:8]2[O:9][C:10](Br)([C:14]([O:16][CH2:17][CH3:18])=[O:15])[CH:11](Br)[O:12][C:7]=2[CH:6]=1)(=[O:3])[CH3:2].[I-].[K+]>CC(C)=O>[C:1]([O:4][C:5]1[CH:21]=[CH:20][C:8]2[O:9][C:10]([C:14]([O:16][CH2:17][CH3:18])=[O:15])=[CH:11][O:12][C:7]=2[CH:6]=1)(=[O:3])[CH3:2]

Komponenten

4

Edukt 2

HCID 4875Potassium IodideHCID 18976125HCID 18976125, Verbindung

Produkt 1

HCID 11043631HCID 11043631, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 180AcetoneLösungsmittel

Versuchsvorschrift

Under an inert atmosphere, 6 g of ethyl 6-acetoxy-2,3-dibromo- 1,4-benzodioxane-2-carboxylate in solution in 100 ml of acetone are mixed with 7.75 g of potassium iodide and stirred for 6 hours. After evaporation of the acetone under reduced pressure, the residue is diluted in ether and then washed with 20% sodium thiosulfate solution until the mixture is decolorized. The organic phase is then dried over magnesium sulfate and thereafter concentrated under vacuum. The compound is purified by chromatography on silica gel (eluent: petroleum ether/ethyl acetate, 7:3).

Aufarbeitung

  1. customAfter evaporation of the acetone under reduced pressure
  2. additionthe residue is diluted in ether
  3. washwashed with 20% sodium thiosulfate solution until the mixture
  4. dry with materialThe organic phase is then dried over magnesium sulfate
  5. concentrationconcentrated under vacuum
  6. customThe compound is purified by chromatography on silica gel (eluent: petroleum ether/ethyl acetate, 7:3)

Quellen und Nachweise

ORD-Eintrag
ord-a6f00ac1b3844fbdb885f65865435152
Quelldatensatz
uspto-grants-1998_09
Patentnummer
US05807882

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