반응 #5298

반응 방정식

p-toluenesulfonic acid

monomethyl ether

( A )

1,6-hexanediol monomethyl ether

acrylic acid

→

1,6-hexanediol monomethyl ether acrylate

용매

water

toluene

반응 조건

후처리

1. 1
   기타was collected
2. 2
   기타were 95°-98° C.
3. 3
   기타nitrogen sparge in vacuo
4. 4
   세척On completion, the product was washed
5. 5
   workup.ADDITION900 ppm p-methoxyphenol (MEHQ) was added
6. 6
   기타the solvent removed at 80° C. with maximum vacuum in the presence of an air
7. 7
   기타sparge
8. 8
   여과Filter aid
9. 9
   workup.ADDITIONwas added
10. 10
    여과the product filtered at 60° C.
11. 11
    기타to give a clear, yellow liquid
12. 12
    기타thermometer, Dean-Stark condenser and sparge tube

실험 절차

803.6 grams of the monomethyl ether described in Part (A) above were azeotropically esterified with 629.8 grams acrylic acid in 254.6 grams toluene in the presence of 24 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. 900 ppm p-methoxyphenol (MEHQ) was added and the solvent removed at 80° C. with maximum vacuum in the presence of an air sparge. Filter aid was added and the product filtered at 60° C. to give a clear, yellow liquid having a viscosity of 6.5 cps and a Gardener color of 3. Equipment used was a 2 liter flask, thermometer, Dean-Stark condenser and sparge tube.

출처