Sulfuric Acid → methyl (2-oxopropoxy)acetate
Reaktionsgleichung
[CH2:1]([O:4][CH2:5][C:6]([O:8][CH3:9])=[O:7])[C:2]#[CH:3].S(=O)(=O)(O)[OH:11]>CO.C([O-])(=O)C.[Hg+2].C([O-])(=O)C>[O:11]=[C:2]([CH3:3])[CH2:1][O:4][CH2:5][C:6]([O:8][CH3:9])=[O:7]Komponenten
5
Edukt 2
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 2
Versuchsvorschrift
The product from Example 1A (56 g, 0.44 mol) in methanol (1.5 L) was treated with mercury(II) acetate (14 g, 44 mmol), treated with concentrated sulfuric acid (3 mL), refluxed for 1 hour, allowed to cool to ambient temperature, concentrated to a volume of 200 mL, treated with 1M HCl (500 mL) and extracted with dichloromethane (thrice, 300 mL). The combined dichloromethane layers were dried (MgSO4), filtered, concentrated and distilled (65-95° C. at 1 torr) to provide the title compound.
Aufarbeitung
- temperaturerefluxed for 1 hour
- concentrationconcentrated to a volume of 200 mL
- additiontreated with 1M HCl (500 mL)
- extractionextracted with dichloromethane (thrice, 300 mL)
- dry with materialThe combined dichloromethane layers were dried (MgSO4)
- filtrationfiltered
- concentrationconcentrated
- distillationdistilled (65-95° C. at 1 torr)
Quellen und Nachweise
- ORD-Eintrag
- ord-2465d680036b4727a5e734aee66f20ce
- Quelldatensatz
- uspto-grants-2003_10
- Patentnummer
- US06632418B2
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