Water → Mono-methoxy diethylene glycol monoacrylate

HRID 5203

반응식

HRID 5203 반응식
[CH3:1][O:2][CH2:3][CH2:4][O:5][CH2:6][CH2:7][OH:8].[C:9]([OH:13])(=[O:12])[CH:10]=[CH2:11].C1(C)C=CC(S(O)(=O)=[O:21])=CC=1.O>C1(C)C=CC=CC=1>[C:9]([OH:13])(=[O:12])[CH:10]=[CH2:11].[CH3:1][O:2][CH:3]([OH:21])[CH2:4][O:5][CH2:6][CH2:7][OH:8]

참가 물질

6

반응물 4

HCID 962WaterHCID 6101p-Toluenesulfonic acidHCID 6581Acrylic AcidHCID 8134Diethylene Glycol Monomethyl Ether

생성물 1

HCID 87063345Mono-methoxy diethylene glycol monoacrylate

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

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.

후처리

  1. customwas collected
  2. customwere 95°-98° C.
  3. customnitrogen sparge in vacuo
  4. washOn completion, the product was washed
  5. addition1,300 ppm p-methoxyphenol were added
  6. customsolvent removed at 80° C. at maximum vacuum with an air
  7. customsparge
  8. filtrationFilter aid
  9. additionwas added
  10. filtrationthe product filtered to clarity at 50° C

출처 및 근거

ORD 기록
ord-0490a3c74fb84af38fee37a9f0e79743
출처 데이터셋
uspto-grants-1993_09
특허 번호
US05243085

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