반응 #73913

ord-86a7fd1f597e4bcc9be765c5275b9823

반응 조건

온도
130°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

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

실험 절차

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.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08541448B2uspto-grants-2013_09