Reaktion #1738677

Reaktionsgleichung

acrylic acid

1-allyloxy-2-propanol

sodium persulfate

isopropanol

→

Acrylic Acid 1-allyloxy-2-propanol

Lösungsmittel

water

water

Reaktionsbedingungen

Aufarbeitung

1. 1
   SonstigeA suitable reaction flask was equipped with a mechanical agitator
2. 2
   workup.ADDITIONa thermometer, a reflux condenser, a nitrogen inlet and two addition inlets for the initiator and monomer solutions
3. 3
   TemperaturThe resulting solution was then heated
4. 4
   Temperaturto reflux under a nitrogen blanket
5. 5
   Sonstigeto provide a mixed monomer solution
6. 6
   SonstigeThe mixed monomer solution was then transferred to an addition funnel
7. 7
   Sonstigewas prepared separately
8. 8
   Sonstigesparged with nitrogen
9. 9
   workup.ADDITIONThe initiator solution (17 g) was then added to the reaction flask along with the mixed monomer solution over a period of two hours
10. 10
    workup.ADDITIONAfter this addition
11. 11
    workup.ADDITIONsome addition persulfate solution
12. 12
    workup.ADDITIONwas added to the reaction mixture for one more hour at 85° C.
13. 13
    workup.ADDITION36 g of 50% caustic solution was then added

Vorschrift

A suitable reaction flask was equipped with a mechanical agitator, a thermometer, a reflux condenser, a nitrogen inlet and two addition inlets for the initiator and monomer solutions. The flask was charged with 170 g of deionized water and 30 g of isopropanol. The resulting solution was then heated to reflux under a nitrogen blanket. 43.2 g of acrylic acid (0.6 mole) and 23.2 g of 1-allyloxy-2-propanol [AOP] (94% pure, 0.19 mole) were mixed in a separate flask so as to provide a mixed monomer solution. The mixed monomer solution was then transferred to an addition funnel. An initiator solution containing 24.4% of sodium persulfate in deionized water was prepared separately and sparged with nitrogen. The initiator solution (17 g) was then added to the reaction flask along with the mixed monomer solution over a period of two hours. After this addition, some addition persulfate solution was added to the reaction mixture for one more hour at 85° C. and, subsequently, 90.0 g of the isopropanol/water solution were stripped off. The reaction mixture was then cooled to lower than 40° C. and 36 g of 50% caustic solution was then added.

Quelle