تفاعل #93666

معادلة التفاعل

N-dichloroacetylpiperid-4-one

propane-1,3-diol

trimethylchlorosilane

→

N-dichloroacetyl-piperid-4-one propylene ketal

المردود 66.6%

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةunder reflux for 12 hours
2. 2
   تركيزThereafter, 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
   أخرىThe resulting brown oil, which slowly crystallized completely
5. 5
   أخرىwas recrystallized from 200 ml of toluene

الإجراء التجريبي

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.

المصدر