Toluene → Alpha-Methylene Phenylethyl Alcohol Methallyl Ether

HRID 622621

Reaktionsgleichung

Reaktionsgleichung von HRID 622621
[OH-].[Na+].C=[C:4]([C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1)[CH2:5][OH:6].Cl[CH2:14][C:15]([CH3:17])=[CH2:16].[C:18]1(C)C=CC=CC=1>>[CH2:17]([O:6][C:5](=[CH2:18])[CH2:4][C:7]1[CH:8]=[CH:9][CH:10]=[CH:11][CH:12]=1)[C:15](=[CH2:16])[CH3:14]

Komponenten

5

Versuchsvorschrift

Into a 3 liter reaction flask equipped with stirrer, thermometer, reflux condenser, addition funnel and heating mantle is placed 240 grams of a 50% aqueous solution of sodium hydroxide; 15 grams of ALIQUAT®336 and 200 ml toluene. The resulting mixture is heated to reflux and over a period of ten minutes, 268 grams of beta-methylene phenylethyl alcohol having the structure: ##STR155## is added followed by addition of 190 grams of 3-chloro-2-methyl-propene over a 25 minute period while refluxing the reaction mass at 104°-110° C. The reaction mass is then continued to be refluxed at a temperature of between 95° and 110° C. for a period of eleven hours. At the end of the eleven hour period, the reaction mass is washed with water. The organic phase is then distilled on a 10" Goodloe column yielding the following fractions:

Aufarbeitung

  1. customInto a 3 liter reaction flask
  2. customequipped with stirrer
  3. temperaturethermometer, reflux
  4. additioncondenser, addition funnel
  5. temperatureheating mantle
  6. temperatureThe resulting mixture is heated
  7. temperatureto reflux and over a period of ten minutes
  8. temperaturewhile refluxing the reaction mass at 104°-110° C
  9. temperatureto be refluxed at a temperature of between 95° and 110° C. for a period of eleven hours
  10. washAt the end of the eleven hour period, the reaction mass is washed with water
  11. distillationThe organic phase is then distilled on a 10" Goodloe column
  12. customyielding the following fractions

Quellen und Nachweise

ORD-Eintrag
ord-e1e46e6a3a9b4b93ae5f464e28ce03c3
Quelldatensatz
uspto-grants-1988_09
Patentnummer
US04772583

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