反应详情

温度

65 °C

In a glass reaction flask was placed 100 g tetradecyl dimethylamine and 0.5 g diethylenetriamine pentaacetic acid. Carbon dioxide sparge into the liquid phase was started and the mixture was stirred and heated to 65° C. The CO2 sparge was stopped and a CO2 gas phase was maintained over the reaction mixture. Dropwise feed of 70 weight percent aqueous hydrogen peroxide was started. At the same time, addition of ethyl acetate was commenced. After 10 minutes all the hydrogen peroxide and 28 mL of ethyl acetate had been added. Cooling was required to maintain the temperature under 75° C. Heat was applied and the reaction continued for two more hours. Dropwise addition of ethyl acetate was continued for the first 19 minutes of the two-hour period. Total ethyl acetate feed was 43 mL. The reaction mixture was a clear gel-free solution. The reaction mixture was analyzed by NMR showing a 100 percent amine conversion. The reaction mixture was poured into a flask containing 300 mL of ethyl acetate and cooled to 15° C. Needle-like crystals of tetradecyl dimethylamine oxide dihydrate formed (106 g) indicating a 87 percent yield.

1. customIn a glass reaction flask
2. customCarbon dioxide sparge into the liquid phase
3. customThe CO2 sparge
4. temperaturea CO2 gas phase was maintained over the reaction mixture
5. additionAt the same time, addition of ethyl acetate
6. additionAfter 10 minutes all the hydrogen peroxide and 28 mL of ethyl acetate had been added
7. temperatureCooling
8. temperatureto maintain the temperature under 75° C
9. temperatureHeat
10. additionDropwise addition of ethyl acetate
11. customwas continued for the first 19 minutes of the two-hour period
12. additionThe reaction mixture was poured into a flask
13. additioncontaining 300 mL of ethyl acetate
14. temperaturecooled to 15° C