Реакция #63783

Уравнение реакции

glycidol

glycidol

H2SO4

H2SO4

glycidol

H2SO4

glycidol

DMAPMA

→

Methacrylamidopropyldimethyl-2,3-dihydroxypropylammonium sulfate

Растворители

water

water

Условия реакции

Обработка

1. 1
   Другоеare 11.2° and 23.1° C.
2. 2
   workup.ADDITIONTwo addition funnels
3. 3
   ТемператураTemperature is maintained between 19.5° and 27.5° C.
4. 4
   ТемператураThe pH is maintained between 10.6 and 11.2
5. 5
   workup.ADDITIONthe remainder is added to the addition funnel
6. 6
   Другоеis removed
7. 7
   Другоеreplaced with a warm water bath in order
8. 8
   workup.ADDITIONThe remaining acid and water mixture is added to the reaction vessel over a period of 2 hours and 41 minutes
9. 9
   workup.ADDITIONDuring this stepwise addition the temperature
10. 10
    Другоеis held at about 40° C.
11. 11
    Температураthe pH is maintained between 11.3 and 10.1 until the last portion of acid
12. 12
    workup.ADDITIONis added
13. 13
    Другоеsubmerged in a 42° C.
14. 14
    ДругоеThe reaction mixture is removed at 16 hours
15. 15
    Другоеat room temperature

Методика

To a 1-liter glass beaker containing a magnetic stirrer is added 170.26 g (1 mole) of DMAPMA and 170.26 g of deionized water while stirring. Initial pH and temperature are 11.2° and 23.1° C., respectively. Two addition funnels are suspended above the beaker; one contains 75.6 g (1 mole) of glycidol and the other contains 98.2 g of 50% H2SO4. The pH and temperature are monitored continuously during the drop-wise addition of glycidol. Temperature is maintained between 19.5° and 27.5° C. by placing the beaker in an ice bath. The pH is maintained between 10.6 and 11.2 by adding 50% H2SO4 as needed. All of the glycidol is added within 1 hour and 4 minutes. An additional 75.6 g of water is added to the reaction mixture; a portion is flowed through the addition funnel which contained the glycidol and the remainder is added to the addition funnel containing the remaining H2SO4. The ice bath surrounding the reaction vessel is removed and replaced with a warm water bath in order to raise the reaction temperature to 40° C. The remaining acid and water mixture is added to the reaction vessel over a period of 2 hours and 41 minutes. During this stepwise addition the temperature is held at about 40° C. and the pH is maintained between 11.3 and 10.1 until the last portion of acid is added. The final pH is 4.55. The reaction mixture is then placed in a sealed brown bottle and submerged in a 42° C. bath. The reaction mixture is removed at 16 hours. The final pH of the product is 5.2 at room temperature.

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