Glycosyl-contained surface active agent as well as preparation method and measuring method thereof
A surfactant, ethylenediamine technology, applied in the preparation of sugar derivatives, surface tension analysis, chemical instruments and methods, etc., can solve the problem of less application of stearyl alcohol, and achieve the effect of improving the reaction yield and reducing the difficulty
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Embodiment 1
[0034] Sodium borohydride (18.9 g, 0.5 mol) and zinc chloride (34 g, 0.25 mol) were added to 250 ml of dewatered tetrahydrofuran and stirred overnight to obtain a light pink slightly transparent solution.
[0035] Stearic acid (71.3 g, 0.5 mol) was added into the bottle, and the temperature was raised until the stearic acid melted. The above-mentioned tetrahydrofuran solution of zinc borohydride was slowly added dropwise, and a large amount of hydrogen was generated. The temperature was maintained at reflux of THF until all 130 ml of solution had been added. The reaction was continued for 4 hours while maintaining the temperature. The system temperature was cooled to room temperature, and a small amount of 1mol / L hydrochloric acid solution was added to quench the excess zinc borohydride. When no gas was produced, an excess of anhydrous potassium carbonate was added. The mixture was allowed to stand overnight, the organic layer was decanted, and the tetrahydrofuran was remov...
Embodiment 2
[0037] Add the stearyl alcohol (126g) and red phosphorus (4g) obtained through the above reduction into the bottle, and raise the temperature to 80°C until the stearyl alcohol melts. Bromine (43.8 g) was slowly added dropwise with stirring. Continue to react for two hours after the dripping. After the reaction, 50ml of petroleum ether was added to the system, and excess red phosphorus was filtered off. The filtrate was first washed with 50ml of 3 sodium sulfite solution, and then dried over anhydrous magnesium sulfate. Petroleum ether was removed under reduced pressure, and the residue was distilled under reduced pressure to obtain octadecane bromide as a light yellow transparent liquid, which became a waxy solid after cooling (186°C, 10mmHg). Yield: 78.5%
Embodiment 3
[0042] Bromooctadecane (42.1 g), ethylenediamine (36 g) and 150 ml of absolute ethanol were stirred at 50° C. for 48 hours. The system was cooled to 30°C, sodium hydroxide (5 g) was added, and stirring was continued for two hours. Salts and excess sodium hydroxide were filtered off, and ethanol was removed under reduced pressure. The residue was washed with water first, and then recrystallized three times with ethanol and petroleum ether to obtain the product as a white solid. Yield: 42.7%
[0043] Mass spectrometer ESI(M+1) + : 313.3
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