Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Hydrogen Peroxide | HCID 784 | — |
| Edukt | Diethylenetriaminepentaacetic acid | HCID 3053 | — |
| Edukt | N,N-Dimethyltetradecylamine | HCID 8211 | — |
| Lösungsmittel | Ethyl Acetate | HCID 8857 | — |
| Produkt | Tetradecyldimethylamine oxide dihydrate | HCID 21983433 | — |
Reaktionsschritte
In a 250 milliliter glass reaction flask was placed 100 grams of tetradecyldimethylamine (0.41 mole; amine value 230.0 mg KOH/g amine) and 0.5 gram (1.27 mmol) of diethylenetriaminepentaacetic acid. This was heated with stirring to 65° C. and then 23 grams (0.47 mole) of 70 weight percent aqueous hydrogen peroxide was added dropwise over a 15-minute period. The mixture was then heated to 76° C. and stirred at that temperature for seven hours. As needed, ethyl acetate (34 mL) was added dropwise to the reaction mass in order to maintain a clear, gel-free liquid. Analysis of the crude reaction mass showed 99 percent amine conversion by proton NMR. The crude reaction mass was added to 400 mL additional ethyl acetate. The solution was then cooled to 15° C. forming a non-hydroscopic white crystalline solid tetradecyldimethylamine oxide dihydrate in 86% recovered yield melting at about 41° C.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patentnummer | US05055233 |
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| Quelldatensatz | uspto-grants-1991_10 |
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| ORD ID | ord-7144b3b5aef5448aa3ea3d6c58be61c5 |
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| Quellennotiz | uspto-grants-1991_10 |
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