2-Tert-Butylphenol → 1-Tert-butyl-2-(methoxymethoxy)benzene
Reaktionsgleichung
[H-].[Na+].[CH3:3][O:4][CH2:5]Cl.[C:7]([C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][C:12]=1[OH:17])([CH3:10])([CH3:9])[CH3:8]>CN(C)C=O>[C:7]([C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][C:12]=1[O:17][CH2:3][O:4][CH3:5])([CH3:10])([CH3:8])[CH3:9]Komponenten
5
Edukt 3
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 1
Reaktionsbedingungen
- Temperatur
- 0 °C
Versuchsvorschrift
Sodium hydride (214 g, 4.90 mol) and chloromethyl methyl ether (394 g, 4.90) were gradually added to a solution of 2-tert-butylphenol (700 g, 4.67 mol) in dimethylformamide (3000 ml) while cooling on ice and the mixture was stirred at 0° C. for 2 hours. The reaction mixture was poured into ice water and extracted with ethyl acetate, and then the organic layer was washed with water and brine in that order and dried over anhydrous magnesium sulfate. The organic layer was concentrated under reduced pressure and the residue was purified by silica gel column chromatography (solvent: n-hexane-ethyl acetate) to yield the title compound (1013 g) as a light yellow oil.
Aufarbeitung
- temperaturewhile cooling on ice
- extractionextracted with ethyl acetate
- washthe organic layer was washed with water and brine in that order
- dry with materialdried over anhydrous magnesium sulfate
- concentrationThe organic layer was concentrated under reduced pressure
- customthe residue was purified by silica gel column chromatography (solvent: n-hexane-ethyl acetate)
Quellen und Nachweise
- ORD-Eintrag
- ord-129a919f9dbc416c91bb4bc243c5eb66
- Quelldatensatz
- uspto-grants-2007_07
- Patentnummer
- US07244730B2
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