Реакция #94989

ord-8c829510ec454091a79435c000eadee9

Реагенты

Нет

Условия реакции

Температура
115°CELSIUS
Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    ДругоеInto a 2 liter reaction vessel
  2. 2
    Другоеequipped with stirrer
  3. 3
    Температураthermometer, heating mantle and overhead condenser with azeotrope takeoff apparatus
  4. 4
    Температураmaintained at a temperature in the range of 104°-127° C.
  5. 5
    Температураat reflux
  6. 6
    Другоеwhile azeotropically removing 80 ml water
  7. 7
    ДругоеAt the end of the 3 hour period
  8. 8
    Другое180° C.

Методика

Into a 2 liter reaction vessel equipped with stirrer, thermometer, heating mantle and overhead condenser with azeotrope takeoff apparatus is placed 488 grams of betaphenylethyl alcohol; 440 grams of cyclohexanol and 100 grams of concentrated sulfuric acid. The reaction mass is then heated to a temperature of 115° C. and maintained at a temperature in the range of 104°-127° C. at reflux while azeotropically removing 80 ml water, for a period of 3 hours. At the end of the 3 hour period, a sample is analyzed by means of GLC analysis (conditions: 180° C. isothermal using an SE-30 packed column). FIG. 1A is the GLC profile of the reaction product at this point.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US04343791uspto-grants-1982_08