Reaktion #93666

Reaktionsgleichung

N-dichloroacetylpiperid-4-one

propane-1,3-diol

trimethylchlorosilane

→

N-dichloroacetyl-piperid-4-one propylene ketal

Ausbeute 66.6%

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturunder reflux for 12 hours
2. 2
   EinengenThereafter, the reaction mixture was concentrated under reduced pressure
3. 3
   workup.DISTILLATIONthe residue was then subjected to brief incipient distillation under greatly reduced pressure
4. 4
   SonstigeThe resulting brown oil, which slowly crystallized completely
5. 5
   Sonstigewas recrystallized from 200 ml of toluene

Vorschrift

A mixture of 19 g (0.09 mol) of N-dichloroacetylpiperid-4-one, 7.5 g (0.099 mol) of propane-1,3-diol and 22.4 g (0.21 mol) of trimethylchlorosilane was boiled under reflux for 12 hours, while stirring. Thereafter, the reaction mixture was concentrated under reduced pressure and the residue was then subjected to brief incipient distillation under greatly reduced pressure. The resulting brown oil, which slowly crystallized completely, was recrystallized from 200 ml of toluene. 16 g (66.6% of theory) of N-dichloroacetyl-piperid-4-one propylene ketal of melting point 115° C. were obtained.

Quelle