反応 #73913

反応方程式

2-(2-bromoethyl)isoindoline-1,3-dione

triethyl phosphite

→

diethyl 2-(1,3-dioxoisoindolin-2-yl)ethylphosphonate

反応条件

後処理

1. 1
   その他Into a 50-mL round-bottom flask purged
2. 2
   温度maintained with an inert atmosphere of nitrogen
3. 3
   濃縮The resulting mixture was concentrated under vacuum
4. 4
   その他The crude product was re-crystallized from ether:n-hexane (1:2)
5. 5
   その他This resulted in 5 g (48%) of diethyl 2-(1,3-dioxoisoindolin-2-yl)ethylphosphonate as a white solid

実験手順

Into a 50-mL round-bottom flask purged and maintained with an inert atmosphere of nitrogen, was placed 2-(2-bromoethyl)isoindoline-1,3-dione (8 g, 31.50 mmol, 1.00 equiv) and triethyl phosphite (6.2 g, 37.35 mmol, 1.19 equiv). The resulting solution was stirred for 18 h at 130° C. The resulting mixture was concentrated under vacuum. The crude product was re-crystallized from ether:n-hexane (1:2). This resulted in 5 g (48%) of diethyl 2-(1,3-dioxoisoindolin-2-yl)ethylphosphonate as a white solid.

出典