反应详情

温度

95 °C

A 1 liter round bottom flask equipped with a thermometer, agitator, condenser, nitrogen inlet tube, and slow addition funnels was charged with a solution of 10 g. water, 20.0 g. sodium vinyl sulfonate (as a 25% solution), 0.8 g. sodium persulfate, and 0.20 g. acrylic acid (Charge A). The contents were purged subsurface with nitrogen for 1 hour while heating to 95° C. The following charges were slowly and separately added over 4 hours: 94.8 g. acrylic acid and 60.0 g. isopropanol (99%) (Charge B) and 18 g. water and 3.0 g. sodium persulfate (Charge C). Reflux developed during the additions and was maintained for 1 hour thereafter. The flask was equipped with a Dean-Stark trap, stripping off of the alcohol was begun, and during the stripping 100.0 g. of 50% sodium hydroxide (Charge D) was slowly added over 2.5 hours. The solution was stripped to about 95° C. and 100 parts of alcohol were removed.

1. customA 1 liter round bottom flask equipped with a thermometer, agitator, condenser, nitrogen inlet tube, and slow addition funnels
2. additionwas charged with a solution of 10 g
3. customThe contents were purged subsurface with nitrogen for 1 hour
4. additionseparately added over 4 hours
5. temperatureReflux
6. temperaturewas maintained for 1 hour
7. customThe flask was equipped with a Dean-Stark trap
8. additionof 50% sodium hydroxide (Charge D) was slowly added over 2.5 hours
9. customwas stripped to about 95° C.
10. custom100 parts of alcohol were removed