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

HRID 467350

反応式

HRID 467350 の反応式
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]

参加物

7

反応物 4

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

生成物 1

HCID 146930481,6-Hexanediol monomethyl ether acrylate

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 1140Toluene溶媒

実験手順

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 air 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.

後処理

  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 air
  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

出典と根拠

ORDレコード
ord-5bef2bfa2c1942f391eee98e8d6d6df5
出典データセット
uspto-grants-1992_10
特許番号
US05159119

関連ノート

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