반응 #93666

반응 방정식

N-dichloroacetylpiperid-4-one

propane-1,3-diol

trimethylchlorosilane

→

N-dichloroacetyl-piperid-4-one propylene ketal

수율 66.6%

반응 조건

후처리

1. 1
   온도under reflux for 12 hours
2. 2
   농축Thereafter, 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
   기타The resulting brown oil, which slowly crystallized completely
5. 5
   기타was recrystallized from 200 ml of toluene

실험 절차

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.

출처