Reaktionsgleichung
C(=O)(O)[O-].[Na+].C([O:8][CH2:9][C:10]([CH3:17])=[CH:11][CH2:12][O:13][C:14](=[O:16])[CH3:15])=O.O.Cl>CO.C(OCC)(=O)C>[C:14]([O:13][CH2:12][CH:11]=[C:10]([CH3:17])[CH2:9][OH:8])(=[O:16])[CH3:15]Komponenten
Versuchsvorschrift
Sodium bicarbonate (0.40 g, 4.75 mmol, 10 mol %) was added to a solution of 4-acetoxy-2-methyl-2-buten-1-ol formate (8.18 g, 47.5 mmol) in methanol (40 ml). The mixture was stirred at room temperature for 2 hours. After completion of the reaction, most of the methanol was evaporated under reduced pressure. The resulting reaction mixture was poured into a mixture of ice-cooled water (20 ml) and ethyl acetate (100 ml). The pH of the aqueous layer was adjusted to 5 to 6 with 1N hydrochloric acid, and the ethyl acetate layer was separated. The aqueous layer was extracted with ethyl acetate (50 ml) twice. The ethyl acetate layers were combined and dried over anhydrous sodium sulfate. Evaporation of the ethyl acetate gave 4-acetoxy-2-methyl-2-buten-1-ol (6.69 g, 46.4 mmol; Yield: 97.7%) as an oil.
Aufarbeitung
- customAfter completion of the reaction
- custommost of the methanol was evaporated under reduced pressure
- customThe resulting reaction mixture
- additionwas poured into a mixture of ice-
- customthe ethyl acetate layer was separated
- extractionThe aqueous layer was extracted with ethyl acetate (50 ml) twice
- dry with materialdried over anhydrous sodium sulfate
- customEvaporation of the ethyl acetate
Quellen und Nachweise
- ORD-Eintrag
- ord-ddbec8c1af6b48f9b6d29aa0b38ef018
- Quelldatensatz
- uspto-grants-1996_06
- Patentnummer
- US05527952
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