반응 #94447

반응 방정식

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

sodium

acetic acid

→

2-(2-piperidinylidene)-acetophenone

용매

ethanol

반응 조건

후처리

1. 1
   온도The reaction mixture is then refluxed for 40 minutes
2. 2
   온도After cooling
3. 3
   여과filtered off from the sodium acetate
4. 4
   농축The filtrate is concentrated in the rotary evaporator
5. 5
   workup.DISSOLUTIONthe residue is dissolved in methylene chloride
6. 6
   추출The solution is repeatedly extracted with water
7. 7
   건조the organic phase is dried over sodium sulphate
8. 8
   기타the solvent is evaporated off in the rotary evaporator
9. 9
   기타The oily residue is crystallised from ether/hexane

실험 절차

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°.

출처