反应详情

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.

1. customwas collected
2. customwere 95°-98° C.
3. customnitrogen sparge in vacuo
4. washOn completion, the product was washed
5. addition900 ppm p-methoxyphenol (MEHQ) was added
6. customthe solvent removed at 80° C. with maximum vacuum in the presence of an air
7. customsparge
8. filtrationFilter aid
9. additionwas added
10. filtrationthe product filtered at 60° C.
11. customto give a clear, yellow liquid
12. customthermometer, Dean-Stark condenser and sparge tube