Reaktion #417404

Reaktionsgleichung

KOH

5-hydroxy-2-(4-octyloxyphenyl)pyrimidine

(S)-8-methyldecyl bromide

→

(S)-5-(8-methyldecyloxy)-2-(4-octyloxyphenyl)pyrimidine

Ausbeute 29.7%

Lösungsmittel

ethanol

Reaktionsbedingungen

Aufarbeitung

1. 1
   Sonstigeprepared
2. 2
   Temperaturunder reflux for 6 hours
3. 3
   Temperaturto cool down
4. 4
   Extraktionextracting it with toluene
5. 5
   Waschenwashing the resulting organic layer with 2N-NaOH aqueous solution
6. 6
   Waschenfurther washing with water until the washing water
7. 7
   workup.DISTILLATIONdistilling off low-boiling components in the organic layer
8. 8
   Sonstigerecrystallizing the residue from ethanol

Vorschrift

KOH (0.8 g) was added to a solution of 5-hydroxy-2-(4-octyloxyphenyl)pyrimidine (4 g) dissolved in ethanol (20 ml), followed by adding (S)-8-methyldecyl bromide (3.2 g) prepared according to the method disclosed in the literature (Mol. Cryst. Liq. Cryst., 1984, Vol. 114, pp. 237-247), keeping the mixture under reflux for 6 hours, allowing the resulting material to cool down, extracting it with toluene, washing the resulting organic layer with 2N-NaOH aqueous solution, further washing with water until the washing water became neutral, distilling off low-boiling components in the organic layer and recrystallizing the residue from ethanol to obtain the captioned compound, (S)-5-(8-methyldecyloxy)-2-(4-octyloxyphenyl)pyrimidine (1.8 g). Its phase transition points were as follows: ##STR12##

Quelle