Reaktionsgleichung
[C:1]1([CH2:7][CH2:8][OH:9])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[CH:10]1(O)[CH2:15][CH2:14][CH2:13][CH2:12][CH2:11]1.S(=O)(=O)(O)O>>[CH:10]1([O:9][CH2:8][CH2:7][C:1]2[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=2)[CH2:15][CH2:14][CH2:13][CH2:12][CH2:11]1Komponenten
4
Reaktionsbedingungen
- Temperatur
- 115 °C
Versuchsvorschrift
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.
Aufarbeitung
- customInto a 2 liter reaction vessel
- customequipped with stirrer
- temperaturethermometer, heating mantle and overhead condenser with azeotrope takeoff apparatus
- temperaturemaintained at a temperature in the range of 104°-127° C.
- temperatureat reflux
- customwhile azeotropically removing 80 ml water
- customAt the end of the 3 hour period
- custom180° C.
Quellen und Nachweise
- ORD-Eintrag
- ord-e90629a28906407980b0bf9dd4c3872a
- Quelldatensatz
- uspto-grants-1983_02
- Patentnummer
- US04374746
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