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p-Toluenesulfonic acid → 1,6-Hexanediol monomethyl ether acrylate

HRID 1195196
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HRID 1195196 반응식
COC.[CH3:4][O:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11]O.[C:13]([OH:17])(=[O:16])[CH:14]=[CH2:15].C1(C)C=CC(S(O)(=O)=O)=CC=1>C1(C)C=CC=CC=1.O>[C:13]([O:17][CH2:11][CH2:10][CH2:9][CH2:8][CH2:7][CH2:6][O:5][CH3:4])(=[O:16])[CH:14]=[CH2:15]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 6101p-Toluenesulfonic acidHCID 6581Acrylic AcidHCID 8254Dimethyl EtherHCID 126516996-Methoxyhexan-1-ol

생성물 1

HCID 146930481,6-Hexanediol monomethyl ether acrylate

시약·촉매·용매 2

HCID 962Water용매
HCID 1140
Toluene
용매

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.

후처리

  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

출처 및 근거

ORD 기록
ord-091ea1e405b84ce29de67baa84b1a4ca
출처 데이터셋
uspto-grants-1992_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05110889

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