반응 #2480028

반응 방정식

water

potassium diphenylphosphide

diethyl 4-fluorophenylphosphonate

→

diethyl 4-diphenylphosphinophenylphosphonate

수율 82.0%

용매

THF

Phosphorus Sulfur

THF

반응 조건

후처리

1. 1
   기타prepared
2. 2
   workup.STIRRINGstirring for 15 min
3. 3
   추출After extraction with ethyl acetate
4. 4
   건조drying the organic phase over Na2SO4
5. 5
   농축the mixture is concentrated on a rotary evaporator

실험 절차

25.8 ml (12.9 mmol) of potassium diphenylphosphide solution in THF (manufacturer: Aldrich) are added dropwise at -5° C. to a solution of 3.09 g (13.2 mmol) of diethyl 4-fluorophenylphosphonate, prepared as described in Phosphorus Sulfur 1980, 9(2), 197.202, in 20.0 ml of THF. After stirring for 19 hours at 23° C., the mixture is hydrolyzed by adding 20 ml of degassed water and stirring for 15 min. After extraction with ethyl acetate, and drying the organic phase over Na2SO4, the mixture is concentrated on a rotary evaporator. 4.20 g of diethyl 4-diphenylphosphinophenylphosphonate (82% of theory) are obtained in the form of a pale yellow oil.

출처