Reaktion #5299

Reaktionsgleichung

water

Methyl Carbitol

acrylic acid

p-toluenesulfonic acid

→

Mono-methoxy diethylene glycol monoacrylate

Lösungsmittel

toluene

Reaktionsbedingungen

Aufarbeitung

1. 1
   Sonstigewas collected
2. 2
   Sonstigewere 95°-98° C.
3. 3
   Sonstigenitrogen sparge in vacuo
4. 4
   WaschenOn completion, the product was washed
5. 5
   workup.ADDITION1,300 ppm p-methoxyphenol were added
6. 6
   Sonstigesolvent removed at 80° C. at maximum vacuum with an air
7. 7
   Sonstigesparge
8. 8
   FiltrationFilter aid
9. 9
   workup.ADDITIONwas added
10. 10
    Filtrationthe product filtered to clarity at 50° C

Vorschrift

682 grams Methyl Carbitol (diethylene glycol monomethyl ether, Union Carbide) were azeotropically esterified with 598.9 grams acrylic acid in 272 grams toluene in the presence of 22.8 grams p-toluenesulfonic acid and inhibitors until no more water was collected. Conditions were 95°-98° C., nitrogen sparge in vacuo. On completion, the product was washed and neutralized with sodium carbonate. 1,300 ppm p-methoxyphenol were added and solvent removed at 80° C. at maximum vacuum with an air sparge. Filter aid was added and the product filtered to clarity at 50° C. The final product was a clear, light yellow liquid, viscosity 6 cps with a Gardner 1 color.

Quelle