تفاعل #94447

معادلة التفاعل

1-phenyl-2-(2-piperidinylidene)-1,3-butanedione

sodium

acetic acid

→

2-(2-piperidinylidene)-acetophenone

المذيبات

ethanol

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةThe reaction mixture is then refluxed for 40 minutes
2. 2
   درجة الحرارةAfter cooling
3. 3
   ترشيحfiltered off from the sodium acetate
4. 4
   تركيزThe filtrate is concentrated in the rotary evaporator
5. 5
   workup.DISSOLUTIONthe residue is dissolved in methylene chloride
6. 6
   استخلاصThe solution is repeatedly extracted with water
7. 7
   تجفيفthe organic phase is dried over sodium sulphate
8. 8
   أخرىthe solvent is evaporated off in the rotary evaporator
9. 9
   أخرىThe oily residue is crystallised from ether/hexane

الإجراء التجريبي

12.15 g (0.05 mole) of 1-phenyl-2-(2-piperidinylidene)-1,3-butanedione are introduced into a prepared solution of 3.5 g of sodium in 120 ml of ethanol. The reaction mixture is then refluxed for 40 minutes. After cooling, it is neutralised with glacial acetic acid, and filtered off from the sodium acetate. The filtrate is concentrated in the rotary evaporator, and the residue is dissolved in methylene chloride. The solution is repeatedly extracted with water; the organic phase is dried over sodium sulphate, and the solvent is evaporated off in the rotary evaporator. The oily residue is crystallised from ether/hexane to yield 2-(2-piperidinylidene)-acetophenone, m.p. 59°-60°.

المصدر