반응 #155899

ord-5477a329b1b04fd7853d9aa383ddd7bd

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타Into a 250-mL 3-necked round-bottom flask, was placed
  2. 2
    기타at room temperature
  3. 3
    기타at room temperature
  4. 4
    기타at room temperature
  5. 5
    온도The resulting solution was heated
  6. 6
    온도to reflux for 3 hr
  7. 7
    농축The resulting mixture was concentrated under vacuum
  8. 8
    온도cooled with a water/ice bath
  9. 9
    여과The solids were collected by filtration

실험 절차

Into a 250-mL 3-necked round-bottom flask, was placed malononitrile (20.4 g, 309.09 mmol, 1.00 equiv) at room temperature. To the resulting mixture was then added 1,1,1-triethoxyethane (50 g, 308.64 mmol, 1.00 equiv), in portions at room temperature. To the resulting mixture was then added acetic anhydride (72 g, 705.88 mmol, 2.28 equiv), in portions at room temperature. The resulting solution was heated to reflux for 3 hr. The resulting mixture was concentrated under vacuum, then cooled with a water/ice bath. The solids were collected by filtration to yield 2-(1-ethoxyethylidene)malononitrile as a white solid.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08822447B2uspto-grants-2014_09