反应 #73913

ord-86a7fd1f597e4bcc9be765c5275b9823

反应条件

温度
130°CELSIUS
详细条件
See reaction.notes.procedure_details.

后处理

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

实验过程

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.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US08541448B2uspto-grants-2013_09