Triethylamine → p-(1-(Cyclohexylethoxy)ethoxy)styrene p-Hydroxystyrene

HRID 353015

Reaktionsgleichung

Reaktionsgleichung von HRID 353015
[OH:1][C:2]1[CH:9]=[CH:8][C:5]([CH:6]=[CH2:7])=[CH:4][CH:3]=1.C(N([CH2:15][CH3:16])CC)C.[C:17]([O:20][CH2:21][CH3:22])(=O)[CH3:18]>C(OC(C)COC)(=O)C>[CH:16]1([CH2:18][CH2:17][O:20][CH:21]([O:1][C:2]2[CH:9]=[CH:8][C:5]([CH:6]=[CH2:7])=[CH:4][CH:3]=2)[CH3:22])[CH2:15][CH2:4][CH2:3][CH2:2][CH2:9]1.[OH:1][C:2]1[CH:9]=[CH:8][C:5]([CH:6]=[CH2:7])=[CH:4][CH:3]=1

Komponenten

5

Edukt 3

HCID 8471TriethylamineHCID 8857Ethyl AcetateHCID 624534-Vinylphenol

Produkt 1

HCID 86598586p-(1-(Cyclohexylethoxy)ethoxy)styrene p-Hydroxystyrene

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 7946Propylene glycol methyl ether acetateLösungsmittel

Reaktionsbedingungen

Temperatur
25 °C

Versuchsvorschrift

p-Hydroxystyrene (VP-8000, produced by Nippon Soda Co., Ltd.) in an amount of 70 g was dissolved in 320 g of propylene glycol monomethyl ether acetate (PGMEA) with heating, dehydrated by vacuum distillation, and then cooled to 25° C. To this solution, 0.35 g of pyridinium p-toluenesulfonate and 22.4 g of cyclohexane ethanol were added, and further 17.5 g of t-butyl vinyl ether was added at a slow speed. In the resulting mixture, reaction was run for 5 hours at 20° C. Thereafter, the reaction solution was admixed with 0.28 g of triethylamine and 320 ml of ethyl acetate, and washed with 150 ml each of distilled water for three times. Therefrom, the solvent was distilled away, and the residue was concentrated. The thus obtained oil was dissolved in 100 ml of acetone, and poured slowly into 2 liter of distilled water. As a result, a powdery matter separated out. This powdery matter was filtered off and dried to yield 54 g of the desired resin.

Aufarbeitung

  1. temperaturewith heating
  2. distillationdehydrated by vacuum distillation
  3. additionTo this solution, 0.35 g of pyridinium p-toluenesulfonate and 22.4 g of cyclohexane ethanol were added
  4. additionfurther 17.5 g of t-butyl vinyl ether was added at a slow speed
  5. customIn the resulting mixture, reaction
  6. washwashed with 150 ml each of distilled water for three times
  7. distillationTherefrom, the solvent was distilled away
  8. concentrationthe residue was concentrated
  9. dissolutionThe thus obtained oil was dissolved in 100 ml of acetone
  10. additionpoured slowly into 2 liter of distilled water
  11. customAs a result, a powdery matter separated out
  12. filtrationThis powdery matter was filtered off
  13. customdried

Quellen und Nachweise

ORD-Eintrag
ord-931071c8e5724b2eb9cdaa8a6a2eb9a0
Quelldatensatz
uspto-grants-2004_06
Patentnummer
US06749987B2

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