反応 #94447

反応方程式

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

sodium

acetic acid

→

2-(2-piperidinylidene)-acetophenone

溶媒

ethanol

反応条件

後処理

1. 1
   温度The reaction mixture is then refluxed for 40 minutes
2. 2
   温度After cooling
3. 3
   ろ過filtered off from the sodium acetate
4. 4
   濃縮The filtrate is concentrated in the rotary evaporator
5. 5
   workup.DISSOLUTIONthe residue is dissolved in methylene chloride
6. 6
   抽出The solution is repeatedly extracted with water
7. 7
   乾燥the organic phase is dried over sodium sulphate
8. 8
   その他the solvent is evaporated off in the rotary evaporator
9. 9
   その他The oily residue is crystallised from ether/hexane

実験手順

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°.

出典