Propylene Glycol → 1,3-Dioxolane, 4-methyl-2-[2-(methylthio)ethyl]-

HRID 462568Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 462568
[CH2:1]1[CH2:6][CH2:5]CCC1.C1(C)C=C[C:10]([S:13](O)(=O)=O)=CC=1.[CH2:18]([OH:22])[CH:19]([OH:21])[CH3:20].CCCC=S>O>[CH3:20][CH:19]1[CH2:18][O:22][CH:1]([CH2:6][CH2:5][S:13][CH3:10])[O:21]1

Komponenten

6

Edukt 4

HCID 1030Propylene GlycolHCID 6101p-Toluenesulfonic acidHCID 8078CyclohexaneHCID 12463483Butanthial

Produkt 1

HCID 1009271,3-Dioxolane, 4-methyl-2-[2-(methylthio)ethyl]-

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

Into a 100 ml reaction flask equipped with spin bar, reflux condenser, heating mantle and hot plate with magnetic stirring apparatus is placed 5 ml cyclohexane, 0.2 grams para-toluenesulfonic acid and 3.8 grams (0.05 moles) of 1,2-propanediol. Over a period of 8 hours, 3-methylthiopropionaldehyde is added to the reaction mass. The reaction mass is then heated to reflux and during refluxing water of formation is removed. The refluxing continues for a period of 7 hours. At the end of the 7 hour period, the reaction mass is transferred to a separatory funnel and washed with one 50 ml portion of saturated aqueous sodium chloride solution and then dried over anhydrous sodium sulfate, filtered and distilled on a Microvigreux column yielding the following fractions:

Aufarbeitung

  1. customInto a 100 ml reaction flask
  2. customequipped with spin bar
  3. temperaturereflux condenser
  4. temperatureheating mantle
  5. temperatureThe reaction mass is then heated
  6. temperatureto reflux
  7. customis removed
  8. waitThe refluxing continues for a period of 7 hours
  9. customAt the end of the 7 hour period, the reaction mass is transferred to a separatory funnel
  10. washwashed with one 50 ml portion of saturated aqueous sodium chloride solution
  11. dry with materialdried over anhydrous sodium sulfate
  12. filtrationfiltered
  13. distillationdistilled on a Microvigreux column
  14. customyielding the following fractions

Quellen und Nachweise

ORD-Eintrag
ord-dee058d289184193a15c03ac9d87f9af
Quelldatensatz
uspto-grants-1985_05
Patentnummer
US04515966

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