反应详情

温度

65 °C

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 by proton NMR showed 99 percent amine conversion. The crude reaction mass was added to 400 mL additional ethyl acetate. The solution was then cooled to 15° C. forming a non-hygroscopic white crystalline solid tetradecyldimethylamine oxide dihydrate melting at about 41° C. in 86% recovered yield.

1. temperatureThis was heated
2. temperatureThe mixture was then heated to 76° C.
3. stirringstirred at that temperature for seven hours
4. temperatureto maintain a clear, gel-free liquid
5. customAnalysis of the crude reaction mass by proton NMR
6. customThe crude reaction mass
7. temperatureThe solution was then cooled to 15° C.