反応 #93666

反応方程式

N-dichloroacetylpiperid-4-one

propane-1,3-diol

trimethylchlorosilane

→

N-dichloroacetyl-piperid-4-one propylene ketal

収率 66.6%

反応条件

後処理

1. 1
   温度under reflux for 12 hours
2. 2
   濃縮Thereafter, 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
   その他The resulting brown oil, which slowly crystallized completely
5. 5
   その他was recrystallized from 200 ml of toluene

実験手順

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.

出典