Iodine → HCID 19001698, Verbindung

HRID 486941

Reaktionsgleichung

Reaktionsgleichung von HRID 486941
II.[Mg].Br[CH2:5][CH3:6].[C:7]([C:10]1[CH:18]=[CH:17][C:13]2[O:14][CH2:15][O:16][C:12]=2[CH:11]=1)(=[O:9])[CH3:8].[Cl-].[NH4+]>O1CCCC1.O>[O:14]1[C:13]2[CH:17]=[CH:18][C:10]([C:7]([OH:9])([CH2:5][CH3:6])[CH3:8])=[CH:11][C:12]=2[O:16][CH2:15]1

Komponenten

8

Edukt 5

HCID 807IodineHCID 6332Ethyl BromideHCID 25517Ammonium ChlorideHCID 76622AcetopiperoneHCID 5462224Magnesium

Produkt 1

HCID 19001698HCID 19001698, VerbindungAusbeute 95,9 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 962WaterLösungsmittelHCID 8028TetrahydrofuranLösungsmittel2×

Versuchsvorschrift

15 ml of tetrahydrofuran and a catalytic amount of iodine were added to 340 mg of magnesium ribbon to obtain a mixture. 1.59 g of bromoethane was gradually added to the mixture in a stream of nitrogen in such a way that the reaction system was mildly refluxed. The resulting mixture was heated under reflux for 30 minutes and cooled, followed by the addition of a solution of 2 g of 5-acetyl-1,3-benzodioxole in tetrahydrofuran. The obtained mixture was stirred at a room temperature for 20 minutes, followed by the addition of a saturated aqueous solution of ammonium chloride and water. The obtained mixture was extracted with ethyl acetate. The organic layer was washed with a saturated aqueous solution of common salt, dried over ahydrous magnesium sulfate and filtered. The filtrate was distilled to remove the solvent. 2.27 g of the title compound was obtained as a crude oil.

Aufarbeitung

  1. customto obtain a mixture
  2. temperaturewas mildly refluxed
  3. temperatureThe resulting mixture was heated
  4. temperatureunder reflux for 30 minutes
  5. temperaturecooled
  6. extractionThe obtained mixture was extracted with ethyl acetate
  7. washThe organic layer was washed with a saturated aqueous solution of common salt
  8. dry with materialdried over ahydrous magnesium sulfate
  9. filtrationfiltered
  10. distillationThe filtrate was distilled
  11. customto remove the solvent

Quellen und Nachweise

ORD-Eintrag
ord-44fdcdda49cc4857834cd7c72c880d61
Quelldatensatz
uspto-grants-1994_03
Patentnummer
US05292901

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