반응 #445294

반응 방정식

phosphonium

Triphenyl phosphine

ethyl bromoacetate

sodium hydroxide

(ethoxycarbonylmethyl) triphenylphosphonium bromide

→

(ethoxycarbonyl methylene) triphenyl phosphorane

수율 80.0%

용매

water

benzene

반응 조건

후처리

1. 1
   온도The solution was heated at 70° for 2 days
2. 2
   온도cooled
3. 3
   여과filtered
4. 4
   세척The residue was washed with benzene
5. 5
   기타dried
6. 6
   기타to give about 16 g
7. 7
   여과The resulting precipitate was filtered off
8. 8
   세척washed with water
9. 9
   기타dried
10. 10
    기타Crystallisation from ethyl acetate/petroleum spirit

실험 절차

Triphenyl phosphine (13 g.) was dissolved in dry benzene (60 ml.) and ethyl bromoacetate (8.3 g.) was added dropwise. The solution was heated at 70° for 2 days, and then cooled and filtered. The residue was washed with benzene and dried to give about 16 g. of (ethoxycarbonylmethyl) triphenylphosphonium bromide. The phosphonium salt (10 g.) was dissolved in water (250 ml.) and 5% aqueous sodium hydroxide was added dropwise with stirring until the solution became alkaline to litmus. The resulting precipitate was filtered off, washed with water and dried. Crystallisation from ethyl acetate/petroleum spirit gave (ethoxycarbonyl methylene) triphenyl phosphorane as a colourless solid in about 80% yield.

출처