반응 #497674

반응 방정식

isopropyl phosphonic dichloride

THF

vinyl magnesium bromide

NH4Cl

→

diethenyl(propan-2-yl)phosphane oxide

수율 80.0%

반응 조건

후처리

1. 1
   기타A 20 L four-necked round bottom flask fitted with an overhead stirrer
2. 2
   온도flame
3. 3
   기타dried
4. 4
   온도cooled in a stream of nitrogen
5. 5
   추출extracted with dichloromethane (4×1000 L)
6. 6
   세척washed with brine (2×15000 mL)
7. 7
   건조dried over sodium sulfate
8. 8
   농축concentrated in vacuo

실험 절차

A 20 L four-necked round bottom flask fitted with an overhead stirrer and dropping funnel, flame dried and cooled in a stream of nitrogen, was charged with isopropyl phosphonic dichloride (350.0 g, 2173 mmol) in THF (5000 mL). The mixture was cool to −78° C. and vinyl magnesium bromide (5217 mL, 5217 mmol, 1M in THF) was added dropwise over 4 h. The reaction mixture was stirred at −78° C. for additional 30 minutes. After completion, the reaction mixture was poured into cold saturated aqueous NH4Cl (3.5 L) and extracted with dichloromethane (4×1000 L). The organic layers were combined, washed with brine (2×15000 mL), dried over sodium sulfate and concentrated in vacuo to give diethenyl(propan-2-yl)phosphane oxide (250 g, 80%) as light-brown oil.

출처