Reaktionsgleichung
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]1Komponenten
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 anhydrous 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
- customto obtain a mixture
- temperaturewas mildly refluxed
- temperatureThe resulting mixture was heated
- temperatureunder reflux for 30 minutes
- temperaturecooled
- extractionThe obtained mixture was extracted with ethyl acetate
- washThe organic layer was washed with a saturated aqueous solution of common salt
- dry with materialdried over anhydrous magnesium sulfate
- filtrationfiltered
- distillationThe filtrate was distilled
- customto remove the solvent
Quellen und Nachweise
- ORD-Eintrag
- ord-45344b7308bd4bdf8758bd4bd4efbdd3
- Quelldatensatz
- uspto-grants-1992_05
- Patentnummer
- US05110956
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