Sulfuric Acid → 1-ethylcyclohexyl methacrylate
Reaktionsgleichung
[C:1]([OH:6])(=[O:5])[C:2]([CH3:4])=[CH2:3].S(=O)(=O)(O)O.[CH2:12]([C:14]1[CH2:19][CH2:18][CH2:17][CH2:16][CH:15]=1)[CH3:13].[OH-].[Na+]>C1(C)C=CC=CC=1>[C:1]([O:6][C:14]1([CH2:12][CH3:13])[CH2:19][CH2:18][CH2:17][CH2:16][CH2:15]1)(=[O:5])[C:2]([CH3:4])=[CH2:3]Komponenten
Edukt 4
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 1
Reaktionsbedingungen
- Temperatur
- 30 °C
Versuchsvorschrift
A 500 ml flask was flushed with nitrogen to displace the air with nitrogen, and was charged with 43.0 g (0.5 mol) of methacrylic acid, 0.5 g (5 mmol) of sulfuric acid and 100 g of toluene. Separately 110.2 g (1.0 mol) of 1-ethylcyclohexene, prepared by the same procedures as described in Reference Example 3, was dissolved in 100 g of toluene. The obtained solution of 1-ethylcyclohexene in toluene was dropwise added to the content in the flask over a period of about 3 hours, while the content was maintained at a reaction temperature of about 30° C. Then the content was stirred for 15 hours at the same temperature. After completion of the reaction, the residual catalyst was neutralized by adding 40.0 g (50 mmol) of a 5% aqueous sodium hydroxide solution, and the neutralized liquid was washed with an aqueous saturated sodium chloride solution. The thus-obtained organic phase was subjected to column chromatography, and further, analyzed by NMR and mass spectrometry. Thus, 68.6 g (yield: 69.9%) of the object 1-ethylcyclohexyl methacrylate was obtained.
Aufarbeitung
- customA 500 ml flask was flushed with nitrogen
- customAfter completion of the reaction
- washthe neutralized liquid was washed with an aqueous saturated sodium chloride solution
Quellen und Nachweise
- ORD-Eintrag
- ord-4cf8a06265904f65b5aaa52426c8fc81
- Quelldatensatz
- uspto-grants-2004_12
- Patentnummer
- US06833462B2
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